HRID532451

反应详情

EQUATION

反应方程式

HRID 532451 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
65 °C

PROCEDURE

实验过程

Tin(II) chloride dihydrate (74.8 g) was added in portions to a solution of 5-bromo-3-nitrothiophene-2-carboxylic acid methyl ester (21.0 g) in methanol (1 L), and the mixture was stirred at 65° C. for 30 min. The mixture was concentrated and 500 mL of ethyl acetate and 700 mL of Rochelle's salt solution were added to the residue. The mixture was vigorously stirred for 1 h. The organic phase was dried over magnesium sulfate and concentrated. The product with the molecular weight of 236.09 (C6H6BrNO2S) was obtained in this way; MS (ESI): 236 (M+H+).

WORKUP

后处理

  1. concentrationThe mixture was concentrated
  2. addition500 mL of ethyl acetate and 700 mL of Rochelle's salt solution were added to the residue
  3. stirringThe mixture was vigorously stirred for 1 h
  4. dry with materialThe organic phase was dried over magnesium sulfate
  5. concentrationconcentrated
  6. customThe product with the molecular weight of 236.09 (C6H6BrNO2S) was obtained in this way