I found another note.

"3L of freezer stored methanol was placed in ice/salt/water bath and gassed with methylamine until it had gained 350g.
After all the stinks of methylamine production, the gassing was incredibly smooth with almost no smell except for the couple antisuckback/gasing rig carb hole openings. A good bit of bubbles go all the way to the top but then must be absorbed from the surface because no smell escapes and when the carb hole is opened for a fraction of a second the methylamine gas lets you know it. This is no joke. Know what you are doing and be prepared. Methylamine gas requires a fume hood. This was placed in the freezer to chill then put on ice and combined with 400g p2p and all the silica gel on hand, about half a liter. The addition of silica gel caused bubbling and temp increase but the bubbles did not fill the liftie van with methylamine gas or perhaps the ventilation was effective. Not sure what the bubbles were. With strong stirring the silca became completely saturated and some popping was heard. This was left to stir in icewater for ~2hrs. Silica gel was colander filtered for speed and mix placed back in ice/salt/water bath and the addition of 45g NaBH4 was started in 1g, then 2g and finally 5g increments. Work out a system for keeping track of additions because you will need it. This addition took a long time due to the HALO breaks between additions. When finished the mix was left to stir with cooling overnight ~8-10hrs. This was filtered, made pH 3 with 15% HCl and volume reduced by distillation in 3 batches. Solution turned pink and bubbles changed. A substantial amount of fragrant oil steam distilled over. Good thing meth is a tough mofo because the original pH 3 went off the 1 end, incase this is of interest to the MD players. Reaction mix chilled and extracted with ether. Reaction mix made pH 13 with 50% NaOH and tents were pitched at the site of the oil layer. This was chilled in the snow then sep'ed, and then extracted with ether. Oil and ether extracts combined, brined, dried and placed in the snow to chill while the psychokitty inspired anhydrous gassing rig was setup. The solution was gassed and a oil layer started to fall out. Frozen dried acetone was quickly added to ~double volume and gassing continued. 3 crops were obtained. Acetone washed, IPA the water recrystallization followed. 195g (35% molar yield) HCl salt. Fuck that sucks. Drying for the formation or the imine is not trivial. Borohydride reductions are clean and easy."

Well, the lifties are obviously ass clowns for proceeding when they knew that the imine formation would be hindered by the incomplete drying.

I think anyone dreaming of this should follow LabTops warning about the moisture and assure the mix is as dry as you can get it.

I also don't see any harm in adding additional fresh dry silica gel after filtering out the first batch and proceeding with the reduction like in Strike's sodium cyanoborohydride classic. I could be wrong.

Does anybody have anything more to add ? Somewhere I could read some more or pick up some more information? This "recipe" is quite vague at times.

Cheers & thanks in advance

I found another note.

"3L of freezer stored methanol was placed in ice/salt/water bath and gassed with methylamine until it had gained 350g.
After all the stinks of methylamine production, the gassing was incredibly smooth with almost no smell except for the couple antisuckback/gasing rig carb hole openings. A good bit of bubbles go all the way to the top but then must be absorbed from the surface because no smell escapes and when the carb hole is opened for a fraction of a second the methylamine gas lets you know it. This is no joke. Know what you are doing and be prepared. Methylamine gas requires a fume hood. This was placed in the freezer to chill then put on ice and combined with 400g p2p and all the silica gel on hand, about half a liter. The addition of silica gel caused bubbling and temp increase but the bubbles did not fill the liftie van with methylamine gas or perhaps the ventilation was effective. Not sure what the bubbles were. With strong stirring the silca became completely saturated and some popping was heard. This was left to stir in icewater for ~2hrs. Silica gel was colander filtered for speed and mix placed back in ice/salt/water bath and the addition of 45g NaBH4 was started in 1g, then 2g and finally 5g increments. Work out a system for keeping track of additions because you will need it. This addition took a long time due to the HALO breaks between additions. When finished the mix was left to stir with cooling overnight ~8-10hrs. This was filtered, made pH 3 with 15% HCl and volume reduced by distillation in 3 batches. Solution turned pink and bubbles changed. A substantial amount of fragrant oil steam distilled over. Good thing meth is a tough mofo because the original pH 3 went off the 1 end, incase this is of interest to the MD players. Reaction mix chilled and extracted with ether. Reaction mix made pH 13 with 50% NaOH and tents were pitched at the site of the oil layer. This was chilled in the snow then sep'ed, and then extracted with ether. Oil and ether extracts combined, brined, dried and placed in the snow to chill while the psychokitty inspired anhydrous gassing rig was setup. The solution was gassed and a oil layer started to fall out. Frozen dried acetone was quickly added to ~double volume and gassing continued. 3 crops were obtained. Acetone washed, IPA the water recrystallization followed. 195g (35% molar yield) HCl salt. Fuck that sucks. Drying for the formation or the imine is not trivial. Borohydride reductions are clean and easy."

Well, the lifties are obviously ass clowns for proceeding when they knew that the imine formation would be hindered by the incomplete drying.

I think anyone dreaming of this should follow LabTops warning about the moisture and assure the mix is as dry as you can get it.

I also don't see any harm in adding additional fresh dry silica gel after filtering out the first batch and proceeding with the reduction like in Strike's sodium cyanoborohydride classic. I could be wrong.

45g NaBH4 for 400g p2p is incorrect.

Phenylacetone, P2P, = 134.18g/mol

Therefore, 400/134.18 = 2.98 moles of P2P.

Sodium borohydride, NaBH4, = 37.83 g/mol

Therefore, 45/37.83 = 1.19 moles of NaBH4.

---

1:1 ratio for sodium borohydride:Phenylacetone

General Procedure for the Reductive Amination of Aldehydes with Methylamine

Titanium(IV)isopropoxide (2 mL, 6.6 mmol) was added to a commercially available solution of methylamine in methanol (2 M, 7.5 mL) followed by the addition of the starting aldehyde (5 mmol). The reaction mixture was stirred at ambient temperature for 5 h, after which sodium borohydride (0.2 g, 5 mmol) was added and the resulting mixture was further stirred for another period of 2 h. The reaction was then quenched by the addition of water (1 mL), the resulting inorganic precipitate was filtered and washed with diethyl ether (20 mL). The organic layer was separated and the aqueous part was further extracted with diethyl ether (2×20 mL). The combined ether extracts were dried (K2CO3) and concentrated in vacuo to give N-methyl secondary amines in high purity.

General Procedure for the Reductive Amination of Ketones with Methylamine

For the reductive amination of ketones, the same general procedure was used except that the combined diethyl ether extracts were next extracted with hydrochloric acid (2 M, 2×10 mL) to separate the neutral materials. The acidic aqueous solution containing the N-methylated amine hydrochloride salt was made alkaline (pH = 10) by slow addition of (10%, w/v) aqueous NaOH and extracted with diethyl ether (2×20 mL). The combined organic extracts were dried (K2CO3) and concentrated in vacuo to give pure N-methylated alkylamines.

http://www.drugs-forum.com/chemistry/chemistry/redamin.ti-nabh4-menh2.html

Good Ref: Imines. page 72. http://www.rohmhaas.com/assets/attachments/industry/pharma_medical/chemical_reagents/reducing_agents/sodium_borohydride_digest.pdf

NaBH4 ammonium acetate + MDP-2-P = frustration

MDP-2-POl is the major product

also it is typical to use about 3 moles of NaBH4 for every mole of substrate because in protic enviroments NaBH4 will decompose and an excess is employed to overcome this.
i think that was the reason for the dismal yeilds in the above example.
it does'nt have to be totally dry because an excess of sodium borohydride will overcome the decomposition
the above example only used one mole.
ammonia is such a shitty nucleophile that the nabh4 reduction gives pitiful yeilds in that scheme.

NaBH4 and MeNH2 in MeOH always gives acceptable yield (60 percent) for MDP2P in not really anhydrous methanol. For MDA you should use commercial NH3 in Methanol to have good yeild.

Vanadium I tried gassing NH3 through methanol, are you sure the yield is better that way then ammonium acetate? I guess it's easier because it's anhydrous, I  could be wrong though

Vanadium I tried gassing NH3 through methanol, are you sure the yield is better that way then ammonium acetate? I guess it's easier because it's anhydrous, I  could be wrong though

It's not because its ahydrous, its because the nitrogen is more nucleophilic. Just look at the species involved