HRID583768

反应详情

EQUATION

反应方程式

HRID 583768 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A 2N aqueous potassium hydroxide solution (16 mL) was added to a stirred solution of 5-methyl-4-(3-benzyl-ureido)-thiophene-2-carboxylic acid methyl ester from Step 2 of Example 16 below (0.4 g, 1.3 mmol) in warm methanol (4 mL), and the mixture was heated under reflux. After 1 hour the mixture was cooled, diluted with water (100 mL), and acidified with aqueous HCl. The precipitate was filtered off, rinsed with water, then ethanol, then ether, and dried to afford 0.29 g of 5-methyl-4-(3-benzyl-ureido)-thiophene-2-carboxylic acid; mp 259-260° C.

WORKUP

后处理

  1. temperaturethe mixture was heated
  2. temperatureunder reflux
  3. temperatureAfter 1 hour the mixture was cooled
  4. filtrationThe precipitate was filtered off
  5. washrinsed with water
  6. dry with materialethanol, then ether, and dried