HRID357300

反应详情

EQUATION

反应方程式

HRID 357300 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of 1.4 g of methyl 2-methyl-4-isopropyl-5-methylsulfonylbenzoate [obtainable by reacting methyl 2-methyl-4-bromo-5-methylsulfonylbenzoate with isopropylzinc chloride in the presence of Pd(II) 1,1'-bis(diphenylphosphine)ferrocene chloride and CuI] and 1.5 g of guanidine in 50 ml of methanol is boiled for five hours and the solvent is then removed. The residue is treated with water and the remaining crystalline crop is filtered off with suction and treated with dil. sodium hydroxide solution. The solid residue is filtered off and recrystallized from ethanol, and N-diaminomethylene-2-methyl-4-isopropyl-5-methylsulfonylbenzamide is obtained, m.p. 220°-223°.

WORKUP

后处理

  1. customthe solvent is then removed
  2. additionThe residue is treated with water
  3. filtrationthe remaining crystalline crop is filtered off with suction
  4. additiontreated with dil. sodium hydroxide solution
  5. filtrationThe solid residue is filtered off
  6. customrecrystallized from ethanol