HRID1631

反应详情

EQUATION

反应方程式

HRID 1631 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
150 °C

PROCEDURE

实验过程

A mixture of 4-chloroisoindoline (700 mg), 2-methylthio-2-thiazoline (600 mg), and β-naphthylsulfonic acid (35 mg) was heated at 150° C. for 30 minutes. The product was cooled, dissolved in methylene chloride, washed with water, the organic layer dried over anhydrous potassium carbonate, filtered, and solvent removed from the filtrate under reduced pressure. The residue was chromatographed on silica gel packed in methylene chloride/2% methanol/ammonia, eluting with methylene chloride/2% methanol, to give 4-chloro-2-(thiazolin-2-yl)isoindoline, a compound of Formula (IA), m.p. 167°-169° C.

WORKUP

后处理

  1. temperatureThe product was cooled
  2. washwashed with water
  3. dry with materialthe organic layer dried over anhydrous potassium carbonate
  4. filtrationfiltered
  5. customsolvent removed from the filtrate under reduced pressure
  6. customThe residue was chromatographed on silica gel
  7. washeluting with methylene chloride/2% methanol