HRID9158

反应详情

EQUATION

反应方程式

HRID 9158 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
20 °C

PROCEDURE

实验过程

A suspension of N-ethyl-N′-(7-oxo-4,5,6,7-tetrahydro-1,3-benzothiazol-2-yl)urea (1.0 g, 4.18 mmol) and thiophenol (0.59 mL, 4.74 mmol) in EtOH (20 mL) was saturated with HCl (g) at about 0° C. The reaction mixture was stirred at about 20° C. for about 2 hrs then a second portion of thiophenol (0.59 mL, 4.74 mmol) was added and the reaction mixture stirred for about another 2 hrs. The ethanol was removed in vacuo and H2O was added. The aqueous phase was neutralized by addition of 2M NaOH and the product was extracted into CH2Cl2 (4 times). The combined organic phases were dried over MgSO4. Evaporation of the solvent gave 1.85 g (quantitative yield) pure product.

WORKUP

后处理

  1. stirringthe reaction mixture stirred for about another 2 hrs
  2. customThe ethanol was removed in vacuo and H2O
  3. additionwas added
  4. additionThe aqueous phase was neutralized by addition of 2M NaOH
  5. extractionthe product was extracted into CH2Cl2 (4 times)
  6. dry with materialThe combined organic phases were dried over MgSO4
  7. customEvaporation of the solvent