Decided against making a new thread for this. I've been researching and getting lots of data together so i can do an almost completely OTC attempt at jon's route (I can get everything here except for the sassy, stuff might bee different in your area) Anyways, I'm just wondering if you wasps can look stuff over, and maybee help me out a bit on some of the math
. Here goes!
---Jon's Route Attempt---
Materials needed:
Safrole
NaBr
Sulfuric Acid
Potassium Iodide
Acetone
Hexamine
IsoHeet
Methanol
Muriatic Acid
Bleach
Vinegar
NaCl
DCM
Epsom Salts
---Chloroform From Bleach and Acetone---
1. Cool bleach
2. mix with acetone
3. wait a couple hours; itll settle to bottom
---Purifying Safrole from Sassy Oil---
1. Mix Sassafras oil with an equal amt of 3% NaOH soln.
2. Pour off (or use sep funnel) water layer
3. Wash 3 more times with distilled water
4. Boil off water on stove; still more alkaloids, but reletively pure
---Methylamine HCl From Hexamine---
1. Make a soln. of 10mols H2O, and 12.8mols of HCl; Remember acid into water!
2. Add this to a beaker with .81mols of hexamine in it. Stir until dissolved
3. Heat on stove/hotplate/whatever; around 80-90c vapors will bee given off, avoid em
4. Heat until you're down to ~200ml, turn off hotplate
5. Let beaker cool until room temp
6. Methylamine HCl will precip out, just filter this off
7. Evap the filtrate until more crystals precip out, and filter again
8. Add the Methylamine HCl to ~100ml of chloroform; supposedly gets out unreacted hexamine, and the dimethylamine
9. Filter off the crystals and keep em dry; mebbe dessicator
---15% conc methylamine from Methylamine HCl---
1. Make a saturated soln of NaOH, and set it to drip into the methylamine HCl
2. Make the gas bubble into dry iso-heet
3. Store in fridge
---GAA from Vinegar---
1.Saturate Distilled vinegar with salt.
2. Extract with DCM (3 times)
3. Dry combined DCM extracts with MgSO4
4. Boil off DCM
---KI from I2 and KOH---
1. Add KOH into KI tincure; Should turn clear
2. Boil down till you have xtals
3. put in oven to dry
---HBr From NaBr and H2SO4---
1. Chill GAA and Sulfuric
2. Take Chilled GAA and add NaBr; make sure it dissolves
3. Add Sulfuric in a steady stream; maybe ice bath to keep down the Br2 gas forming
-*-Bromosafrole from Crude Safrole-*-
1. Take 40% HBr in GAA and mix with safrole
2. Swirl if you want, and put in freezer (0c) for 24 hours
3. After 24hrs put in sep funnel, flood with water
4. get the bromosafrole out
5. extract water layer 3 times with chloroform
6. mix the chloroform and bromosafrole
7. Wash with water and add bicarb until fizzing stops
8. Wash a couple more times with water; ofc discard all previous washes
9. Store Bromosafrole in the fridge.
-**-Iodosafrole from Bromosafrole-**-
1. Dissolve KI into Acetone
2. Add KI soln into Bromo. Let sit for 30-45mins
3. Flood with water until salts dissolve
4. Extract 3 times with DCM
5. Evap DCM with hairdryer
6. Put Iodosafrole in the fridge, also keep away from UV
-***-Freebase(or HCl) MDMA from Iodosafrole-***-
1. Put iodosafrole and 15% methylamine into a sealed container
2. Swirl and let it sit for 30-45 minutes (just to bee safe)
3. Put mixture into Buchner funnel and use water asp to evap the alcohol
4. Make the pH of the mix 12 with NaOH and watch the freebase oil drop out.
5. gas it with a ghetto gas generator for the HCl
Note: Regular "-" is making of precursors, and other materials needed, while "*" is the workup (Safrol->bromo->iodo->fb)
Topic: Jon's route (Read 3445 times)
CV1P0347.pdf
(122.17 kB - downloaded 25 times.)
nothing else done with it yet.
