moved to a new state.156.35g safrole + 2.35g KOH, vac reflux 18h from 120-128°C. separated forerun to 129°C, distil 139.2g isosafrole from 129-133°C.
139.2g isosafrole + 430ml DCM + 27g Na2CO3, mix 204.6g 90% formic, 133.8g 29% H2O2 for 1h w/ cooling. dripped in performic over 1.25h, stirred 34h. strip DCM, (using 124.2g 15% H2SO4, 41.4ml MeOH per 100ml iso) add 1063.9g 15% H2SO4 + 355ml MeOH. reflux 3h, pour off top 750ml, tap off ketone. extract each portion 100ml, 3x 40ml, 20ml DCM. washed ~500ml DCM soln 3x 200ml, 100ml bicarb. added a bit of old ketone, distilled 7.3g forerun from 85-100°C 4x. distilled 110.9g ketone at 102°C while passed out for 5h. cranked heat, caught 10 drops at 116°C before i realized glycol is bad to have in ketone. 72.5% m/m or 77.3% m/m including the forerun.
2 L MeNH2 reaction. from OrgSyn: 18mol CH2O + 13.32mol NH4Cl + ~700ml H2O use 420g HMTA=hexamine, 78g NH4Cl, 450g HCl = 1607.1g 28% HCl. overheated 1h to 106°C, 2h at 100°C, 2h at 103°C, 2h at 100°C, 1h at 102°C. cooled and filtered 357.7g wet NH4Cl which dried to 352.9g 2days later. reduced volume with heat and aspirator vac until 1L, croppped off 114.8g NH4Cl which was stirred with 150-200ml MeOH to add back to the mother liquor. the 114.8g NH4Cl dried to 96.9g then 89.9g. stripped liquids for 19h with aspirator, added 300ml more MeOH and stripped off with any residual H2O for 1h, added 50ml MeOH and repeated. added 1100ml dry IPA, reflux and decant to yield 100g MeNH2.HCl from the first crop after 7-8h filtering time. second crop ~63g in 3h time. third crop 75.3g. forth crop 25.5g. 264g MeNH2.HCl total, with some still unfiltered.
20.6g ketone + 25.7g MeNH2.HCl + 26.7ml H2O + 15.26g NaOH in 28ml H2O. 163ml MeOH, 10.3g Al, dripped in ketone over 30min, reflux 1drop/sec for next 15min, Al gone in 1h more. added 6.2g NaOH in 100ml H2O to pH 14. extracted 100ml, 50,2x 60, 2x 40 toluene (350ml). dried over 19g MgSO4, gassed 2x to yield 18.01g MDMA.HCl
97.6g ketone + 121.75g MeNH2.HCl in 126.5ml H2O + 72.3g NaOH in 227.4ml H2O. 773ml MeOH, 48.8g Al. dripped in ketone over 1h 10min, got hot but failed to reflux, stirred w/ intermittent heat for 4days. added 24.5g NaOH in 425ml H2O. extracted 280ml, 2x 190ml, 100ml toluene. washed 2x 100ml 4x 50ml brine. 760ml toluene picks up 65ml vol with orange color. mixed 47.7g 28% HCl in 150ml H2O, added 125ml which gives pH 1 (ouch). toluene is now 800ml volume. basify the 400ml acqueous extract to pH 12 with NaOH. extract with 225.7g DCM, strip DCM, added toluene (redundantness) and gassed 3.5g MDMA.HCl which went from yellow to orange to brown as gassing was completed. recrystalized once from IPA to yield 2.5g of still-brownish MDMA.
250.9g raw sassy. distil w/ 100mm frac column, aspirator vac. distil forerun to 124-126°C, steel-wool packed-column floods over 1drop/2sec rate. distil 209.65g safrole at 128°C. add 3.15g KOH. vac reflux with aspirator vac from 128°C-139°C over 19h. collected small forerun from 124-128°C, ~5-10g cis-isosafrole from 132-134°C, 3 foreruns to 138°C, then 175.8g trans-isosafrole from 140-146°C (84% yield).
175.8g isosafrole + 543ml DCM + 34.1g Na2CO3. mix 258.4g 90% formic, 169g 29% H2O2, add performic over 1.5h, stir 30h, strip DCM, add 400ml MeOH, 1400g 15% H2SO4. reflux 3h, split in two portions and extract each 100ml, 2x 50ml, 2x 40ml DCM. wash 560+ml DCM soln w/ 200ml, 2x 100ml NaHCO3 soln. distilled some forerun 95-105°C, 30.7g ketone from 105-125°C. 99.2g ketone from 125-135°C. (129.9g total, 67.2% m/m)
20.8g 3rd fraction ketone (from the 99.2g) + 26g MeNH2.HCl + 27ml H2O. 15.4g NaOH + 48.5ml H2O. 165ml MeOH, 10.4g Al (3.3x molar equiv to ketone) ran hot at first but dies suddenly. heated for next 7h. added 5.5g NaOH in 90ml H2O to pH 14. extracted 110, 70, 65, 65ml toluene. (toluene is light yellow, 1/3 of Al is unconverted to Al(OH)3 ). gassed to create orange sludge and 1.8g of light yellow MDMA.HCl (after acetone washing away the orange). without recrystallizing the MDMA turned brown and inactive in just 1-2weeks.
10.1g 2nd fraction ketone (from the 30.7g) + 12.6g MeNH2.HCl in 13.1ml H2O. 7.5g NaOH in 23ml H2O, 80ml MeOH, 5.05g Al. drip in ketone over 20min, drip rate increases slowly for 1h to 1drop/10sec. peak rate is 1drop/6sec. 30min later drip rate is 1drop/30sec and Al is mostly gone. stirred 4.5h total, add 2.6g NaOH in 40ml H2O to pH 14. extract 2x 50ml, 60ml, 35ml toluene. washed 3x 70ml brine, dried over 12.5g MgSO4, gassed 2.75g decent MDMA.HCl
redistilled 2nd ketone fraction- collecting 7.3g from 92-96°C, then 6.1g from 96-100°C.
7.3g fraction 2A ketone + 9.1g MeNH2.HCl in 10ml H2O. 5.4g NaOH in 16.6ml H2O, 60ml MeOH, 3.65g Al. drip in ketone over 20min, flask is hot 30min later, no reflux, stirred 8h, Al is gone. add 1.9g NaOH in 50ml H2O to pH 12. extract 40ml, 25ml, 3x 20ml toluene, dry over 7g MgSO4. no yield at all :<<<<<
6.1g fraction 2B ketone + 2.71g Na2CO3 + 5.14ml H2O + 3g NH2OH.HCl, stir then add ketone + 25.7ml EtOH. reflux 1.5h, add 13.15ml H2O, no oxime falls out of solution, ever.
247.1g raw sassafras. distill with 200ml frac column, collection 31g forerun mostly at 122°C steady. next fraction begins at 128-132°C, switched out a leaking rubber stopper (40ml so far), a few more drops come at 122°C, then the main fraction at 140-142°C 192.6g water-white safrole.
O2 wacker. 50g safrole needs .15mol O2 which equals a 30psi total drop in pressure in the space left in a 2L soda bottle. stir 1g PdCl2 in 150ml ~99% IPA for 2h with 1ml H2O. add 2.8g CuCl2.2H2O, 125ml IPA, .5ml H2O, 50g safrole. pressurized bottle with welding-grade O2 to 35psi.
3x5 min shaking, 5 min heating (warm water) -> 32psi
5 min shaking, 4x10 min rest + 10min shaking -> 30psi
5 min shaking, 4x10 min rest + 10min shaking -> 32.5psi
5 min shaking, 4x10 min rest + 10min shaking -> 33psi
6x5 min heat + 5 min shaking -> 34.5psi
Result = 16psi drop instead of 30psi
added 400ml H2O, cooled, decanted/filtered and extracted 4x 50ml DCM, volume of DCM extracts is 350ml. washed 2x 100ml, 3x 75ml brine giving 225ml DCM extracts (better). collected forerun from 56°C, mostly 85-90°C, to 92°C. distilled 29.4g yellow-green fake ketone (mdp3p probably, the aldehyde) from 94-100°C.
20.1g MDP3P + 25g MeNH2.HCl + 26ml H2O, 14.85g NaOH + 46.7ml H2O, 160ml MeOH, 10g Al. dripped in over 30min, reflux is 1drop/20sec, 1drop/11sec 20min later, 1drop/8sec 10min later, in 5.5h all Al is gone. basified to pH 13 with 5.1g NaOH in 95ml H2O. extract 90, 3x 60ml, 45, 35ml toluene (350ml total). washed, dried, and gassed - no amines at all. obviously.
142.5g 2x distilled safrole + 2.14g KOH, reflux at 5:30am 128°C to 134°C at 9:30am.
After filling out a 'change of address' form to have my mail delivered after a long time without service, some weird fuckers (the FBI) showed up in an unmarked Lexus early in the morning radios crackling to pound on my door like the devil, but never bust in. without a warrant the pigs can't work, not here. scary. sure i had 17 2 inch cannabis seedling in my 3rd floor window which the neighbors could have seen from their window 20 feet across the street. but i don't think it was about anything as simple as my styrafoam cups. what kind of cop would warn a pot-grower to ditch his plants instead of getting a warrant and seizing them. no local cop i know. especially not knocking like that. It was FBI sure enough.
Cleared everything from the house in a few hours, after buying fukkin' tobacco. Moved to a 'friend's house.No heat on the isomerization for 3.5days, heat 12h with fridge compressor vacuum. temp climbs 134-138°C, distilled forerun 123-126°C using 200ml frac column. collected cis-iso starting at 134°C thru tran-iso thru 140°C, 129.9g isosafrole total.
129.9g Isosafrole + 400ml DCM + 25.2g Na2CO3. mix 191g 90% formic + 120.7g 30% H2O2 equiv to 106.81ml 35% H2O2 at 20°C. run 28h, strip DCM 4h without vacuum, 4h with (non-functional) aspirator vacuum. add 1079g 15% H2SO4 + 360ml MeOH. reflux 3h. extract each 750ml portion with 100ml, 2x 50, 2x 25 DCM. wash 3x 200ml, 100ml bicarb soln. distilled sticky ketone from 165-180°C.
redistilled first 30g fraction, collection 5.5g from 100-108°C with fresh oil in the pump. distilled 500ml of 5.6% MeNH2/MeOH solution from saved basic post-methylamination solutions. reduced 5.5g ketone to yield .32g MDMA.HCl. enough to trade for an eighth of ganja.
177.5g safrole + 2.66g KOH, reflux 12h temp goes from 135-145°C. distilled 161.9g isosafrole from 144-148°C. 62.15g isosafrole + 191ml DCM + 12.05g Na2CO3. mix 91.4g 90% formic + 57.7g 30% H2O2 = 50.65ml 35% H2O2 at 0°C. used 58g H2O2 = 52ml. yield 83.9g monoformyl glycol (97.5% m/m)
83.9g monoformyl glycol + 172ml MeOH, 516.3g 15% H2SO4. reflux 3h, extract, wash and distil 47.15g ketone from 117-120(2)C.
10.75g ketone + 5.3g Al + 105g 5.6% MeNH2 soln + 1.5ml H2O. drip ketone in 30min. reflux hard 15min later for ~30min. stirred 5h, added 2.5g NaOH in 120ml H2O to pH 14. extracted 60ml, 40, 32, 30, 20ml toluene. washed 3x 70ml brine, dried 1h over 13g MgSO4. gassed 10g MDMA.HCl
12g ketone + 6g Al + 112g 5.6% MeNH2 + 2ml H2O. stir, then add 3g NaOH in 150ml H2O to pH 14. extract 70ml, 2x 40ml toluene. washed with brine and gassed 9.8g MDMA.HCl (reaction was slow to heat up, characteristic of yellowish ketone that is not totally pure)
25g ketone + 12.5g Al + 334g 3.75% MeNH2 soln + 5ml H2O. basified 11g NaOH in 400ml H2O to pH 12. extracted 100ml, 50, 80, 60, 2x 50ml xylene (390ml). washed 150ml, 2x100ml brine. gassed 21g MDMA.HCl
I know the above ketone amounts don't add to 47.15g, blame my Ohaus scale.
99.75g isosafrole + 306.55ml DCM + 19.4g Na2CO3. 147.06g 90% formic + 92.84g 30% H2O2. ran 30h, stripped DCM, 200ml tap H2O added accidentally by bad aspirator suck-back. decanted H2O to leave 129.9g wet monoformyl glycol (93.5%).
129.9g monoformyl glycol + 266ml MeOH + 800g 15% H2SO4. ran 3h, extract 100ml, 2x 75ml, 2x 50ml DCM (350ml total). distilled forerun from 109-113°C, bulk of ketone at 120°C. first fraction is 50.15g at 120°C, 2nd fraction is 27.1g at 120°C, 3rd fraction is 4.0g from 120-145°C where distillation was stopped. yield 77.25g ketone.
12.4g 2nd fraction ketone + 18g MeNH2.HCl in 18.7ml H2O. 10.0g NaOH in 33.6ml H2O. add 115ml MeOH, 7.2g Al, mercury salt, methylamine, base, ketone & stir 18h. add 4.1g NaOH in 65ml H2O to pH 12. extract 75ml, 55, 50, 47, 50 xylene (277ml). wash, dry over 18g not-so-dry MgSO4.1H2O, gassed 15.06g MDMA.HCl (86.58% m/m)
21.75g 1st fraction ketone + 25.5g MeNH2.HCl in 27.2ml H2O. 14.5g NaOH in 49ml H2O. 180.4ml MeOH, 10.5g MM-ground Al foil. run. add 6.2g NaOH in 100ml H2O to pH 12. extract 100ml, 80, 70, 2x 60, 30 toluene (400ml). wash 4x 100ml brine, gas 19.46g MDMA.HCl
friends ask me to leave their house after a 'repair-man' sent by the 'land-lord' asks to see their kitchen floor for the purpose of replacing it. they tell him to go away and have the landlord call ahead, obviously. my gear is back in my car that morning and in my house the next day. The fear gets intense.12.7g 2nd fraction ketone. add 5.64g Na2CO3 to 10.8ml H2O, heat, add ketone in 53.5ml EtOH, add 6.2g NH2OH.HCl, reflux 2h. add 31ml H2O and cool 12h in freezer. filter and dry overnight to get 10.68g mdp2p oxime.
10.68g oxime + 12.8g Al, 164ml EtOH + 16.6ml H2O, 29.7g HOAc. add 2x 45ml 85% EtOH as necessary. added 34g NaOH in 360ml H2O to pH 14. extract 70ml, 2x 60, 50, 40 toluene (280ml). wash 3x 100ml brine (no emulsions). dry over 18g MgSO4, gas 7.06g MDA.HCl (with some Al unreacted).
Redistilled 28.4g 1st fraction ketone w/ 100m frac column, got 2.7g forerun 84°C-102°C. 1.75g more from 102-114°C. then 20.6g ketone from 110-114°C.
At this point i hear thru the grapevine that the FBI has questioned my friends father whose house he had 5g of shitty brown-red useless PdCl2 sent to. i take it as a good sign that the FBI has few enough resources that they question him instead of surveilling his son and thus finding me. i stopped hanging out with him, until the treasure was properly buried at least.20.6g ketone, 9.15g Na2CO3 + 17.5ml H2O, heat, add ketone, 86.8ml EtOH, 10.05g NH2OH.HCl, reflux 2h, add 50ml H2O, cool, seed and filter after 7h, then filter again 6h later to catch the oxime that slipped thru. yield 22.62g oxime weighed on a Mettler +-1mg.
22.62g oxime + 27.144g Al, 382ml 85% EtOH = 346.8ml EtOH + 35.2ml H2O, amalgamate, add oxime + 62.8g HOAc, add 75ml 85% EtOH during reaction (should have used 150ml as Antibody2). (also should have used good EtOH instead of the orange-store denatured S-L-K shit). stirred 6.5h. add 71g NaOH in 380ml H2O to pH 14 which causes reflux to begin again. poured mother liquor into a 1L beaker, added 60ml H2O to carry the excess AlOH+goodies over. extracted 104ml, 92ml, 79ml, 72ml, 63ml, 52ml, 40ml xylene (492ml total). washed 5x 100ml brine. dry over 32g MgSO4.1H2O. gas 12.4g MDA.HCl. fuck that bad-EtOH nonsense.
The FBI can arrest me now because i have given away all my drugs to people who needed them more than i and all my knowledge to similar folks. then i burned my notebook. Hallelujah god alive.