HRID2255454
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
3-(2-Trifluoroacetylimino-6-trifluoromethoxy-3-benzothiazolinyl)propyl p-toluenesulphonate (3.88 g) and sodium methanethiolate (1.03 g) in absolute ethanol (20 cc) are heated at 60° C. for 6 hours. After cooling to a temperature close to 20° C., the reaction mixture is concentrated to dryness under reduced pressure (20 mm Hg; 2.7 kPa). The oily residue is taken up in distilled water (50 cc) and the organic phase is extracted with ethyl ether (50 cc). After drying over magnesium sulphate and concentrating to dryness under reduced pressure, 2-imino-3-(3-methylthiopropyl)-6-trifluoromethoxybenzothiazoline (1.88 g) is obtained, which is converted to the hydrochloride melting at 181° C.
WORKUP
后处理
- temperatureAfter cooling to a temperature
- customclose to 20° C.
- concentrationthe reaction mixture is concentrated to dryness under reduced pressure (20 mm Hg; 2.7 kPa)
- extractionthe organic phase is extracted with ethyl ether (50 cc)
- dry with materialAfter drying over magnesium sulphate
- concentrationconcentrating to dryness under reduced pressure