反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
To a solution of 2-guanidino-4-(3-aminocyclopentyl)thiazole (0.3 g.) in ethanol (5 ml.) was added methyl isothiocyanate (0.15 g.) and the mixture heated under reflux for 1 hour. The reaction mixture was evaporated to dryness and the residue subjected to preparative thin layer chromatography on silica gel GF plates (Uniplate, Analtech Inc., Delaware, U.S.A.) using chloroform/methanol/aqueous ammonia (s.g. 0.88) 135:15:1 v/v/v for development. The appropriate region of the chromatogram was eluted with warm ethanol/chloroform (3:1 v/v) and the extract evaporated to give 2-guanidino-4-[3-(3-methylthioureido)cyclopentyl]thiazole as a light brown glass. The n.m.r. spectrum in d6 dimethyl sulphoxide included signals at 1.2-2.2 (m) 2.8 (d, 3H) 4.2 (br m, 1H), 6.27 (s, 1H) and 6.78 (br s, 4H).
WORKUP
后处理
- temperaturethe mixture heated
- temperatureunder reflux for 1 hour
- customThe reaction mixture was evaporated to dryness
- washThe appropriate region of the chromatogram was eluted with warm ethanol/chloroform (3:1 v/v)
- customthe extract evaporated