HRID274325

反应详情

EQUATION

反应方程式

HRID 274325 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
90 °C

PROCEDURE

实验过程

5.47 g of ethyl pentanimidoate hydrochloride (J.A.C.S., Vol. 64, p. 1827 (1942)) were added to a solution of 5 g of methyl 3,4-diaminobenzoate in 60 ml of tetrahydrofuran, and the mixture was stirred for 3 hours and 30 minutes at 90° C. The tetrahydrofuran was evaporated off and 50 ml of a saturated solution of sodium bicarbonate were added. The mixture was extracted with methylene chloride and the extracts were washed with water, dried and evaporated to dryness under reduced pressure to obtain 9 g of product which was crystallized from isopropyl ether to obtain 6.65 g of the desired product melting at 114° C.

WORKUP

后处理

  1. customThe tetrahydrofuran was evaporated off
  2. addition50 ml of a saturated solution of sodium bicarbonate were added
  3. extractionThe mixture was extracted with methylene chloride
  4. washthe extracts were washed with water
  5. customdried
  6. customevaporated to dryness under reduced pressure