(Hive Addict)
04-19-03 13:54
No 428040
(Rated as: excellent)
Phloroacetophenone: Place 25.2 g (0.2 mol) of dry phloroglucinol, 16.4 g (20.9 mL, 0.4 mol) of anhydrous acetonitrile, 100 mL of sodium-dried ether and 5 g of finely powred, fused zinc chloride in a 500-mL Buchner flask fitted with a wide gas inlet tube. Protect the side-arm of the flask with a calcium chloride guard tube. Cool the flask in an ice-salt mixture in the fume cupboard and pass a rapid steam of dry HCl (g) through the solution for 2 hours with occasional shaking. Allow the flask to stand in an ice chest for 24 hours, and again pass dry HCl (g) into the pale orange mixture for a further 2 hours. Stopper the flask and leave it in an ice chest (or refrigerator) for 3 days. A bulky orange-yellow precipitate of the ketimine hydrochloride is formed. Decant the ether and wash the solid with two 25 mL portions of anhydrous ether. Transfer the solid with the aid of about 1 litre of hot water to a 2-litre RB flask provided with a reflux condenser. Boil the yellow solution vigorously for 2 hours, allow to cool somewhat, add 4-5 g of decolourising carbon with two 100 mL portions of boiling water and add the filtrate to the main product. Allow to stand overnight, and filter the pale yellow of colourless needles of phloroacetophenone at the pump, dry at 120°C to remove the molecule of water of crystallisation and preserve in a tightly stoppered bottle. The yield is 29 g (85%), m.p. 217-219°C. This product is pure enough for many purposes, but may be obtained absolutely pure by recrystallisation from hot water (35 mL per gram) and drying at 120°C; m.p. 218-219°C.
Reference: Vogel's page 1017 exp 6.125
Never underestimate the power of Vogel's!
Accept No Imitations, There Can Only Bee One; www.the-hive.ws
(Hive Bee)
04-19-03 14:46
No 428049
You keep on doing it pHarmacist ,yep another fine post from you
.Littlejase
.
" Better to be than not to Bee "
(Hive Addict)
04-20-03 22:02
No 428232
Thanks littlejasebee!
Nevertheless, I got a PM from a top-bee claiming that there might bee some confusion as this compound is not mentioned as beeing a TMA-6 precursor anywhere in PiHKAL. Well, that's correct, but acetophenones are well-known amphetamine precursors so I figured it can bee used in acetophenone route to TMA-6 (LOL!). This is a completely different path to TMA-6. It was stupid of me not to point this out when I made the above post.
Accept No Imitations, There Can Only Bee One; www.the-hive.ws
(Hive Bee)
04-20-03 23:16
No 428250
Hi pHarmacist
,Nice post up there, but are you sure acetophenones are useful for the synthesis of amphetamines? Propiophenones are I agree; however, won't acetophenones, with their 2-carbon side chains, only be useful for synthesising PEA derivatives?
(Hive Bee)
04-21-03 16:21
No 428379
If 2,4,6,-trihydroxyacetophenone can be used as precursor for TMA-6, could one use 2,4,5-trihydroxyacetophenone to synthesize TMA-2? And, pHarmacist, if you have some reaction details, could you please post them. Thanks.
I'm dreaming of the white crystals.