HRID2255454

反应详情

EQUATION

反应方程式

HRID 2255454 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. temperatureAfter cooling to a temperature
  2. customclose to 20° C.
  3. concentrationthe reaction mixture is concentrated to dryness under reduced pressure (20 mm Hg; 2.7 kPa)
  4. extractionthe organic phase is extracted with ethyl ether (50 cc)
  5. dry with materialAfter drying over magnesium sulphate
  6. concentrationconcentrating to dryness under reduced pressure