反应详情

Ethyl-m-[N,N-di(n-hexadecyl)aminomethyl]-thiobenzimidate dihydrochloride (1.074 g., 1.5 mmoles) was added to a slurry of 2,2,2-trifluoroethylamine hydrochloride (406 mg., 3.0 mmoles) and anhydrous sodium acetate (246 mg., 3.0 mmoles) in chloroform (10 ml.) and glacial acetic acid (0.3 ml., 5.3 mmoles). The mixture was held for 12 hours at room temperature. It was then diluted to 300 ml. with chloroform, washed with saturated aqueous sodium bicarbonate solution (2 × 50 ml.), washed with saturated aqueous sodium chloride solution (2 × 50 ml.), dried (Na2 SO4) and filtered. The filtrate was acidified with a 10% solution of anhydrous hydrogen chloride in dioxane (5ml.) and then evaporated in vacuo to a foam. The foam was crystallized from 1,2-dimethoxyethane [974 mg., 86% yield, Rf .39 (4:1, benzene: ethanol on silicic acid), m.p.-forms a gel at 125°-127° C.].

1. additionIt was then diluted to 300 ml
2. washwith chloroform, washed with saturated aqueous sodium bicarbonate solution (2 × 50 ml.)
3. washwashed with saturated aqueous sodium chloride solution (2 × 50 ml.)
4. customdried (Na2 SO4)
5. filtrationfiltered
6. customevaporated in vacuo to a foam
7. customThe foam was crystallized from 1,2-dimethoxyethane [974 mg
8. customat 125°-127° C.