HRID1094713

反应详情

EQUATION

反应方程式

HRID 1094713 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of ethyl 5-methyl-4-oxo-3,4-dihydrothieno[2,3-d]pyrimidine-6-carboxylate (1.0 g, 4.5 mmol) in THF (14 mL), MeOH (3 mL), and H2O (3 mL) was added lithium hydroxide monohydrate (0.68 g, 16 mmol). The reaction mixture was stirred at RT overnight. The reaction mixture was concentrated, diluted with H2O (20 mL) and washed with DCM (25 mL). The aqueous layer was acidified (pH˜2) with 1M HCl and the resultant precipitate was filtered and dried to give 0.9 g of pure 5-methyl-4-oxo-3,4-dihydrothieno[2,3-d]pyrimidine-6-carboxylic acid, (yield: 94%).

WORKUP

后处理

  1. concentrationThe reaction mixture was concentrated
  2. additiondiluted with H2O (20 mL)
  3. washwashed with DCM (25 mL)
  4. filtrationthe resultant precipitate was filtered
  5. customdried