HRID2364003

反应详情

EQUATION

反应方程式

HRID 2364003 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

To a stirred suspension of 6-bromo-1,2,2-trimethyl-2,3-dihydrothieno[3,2-d]pyrimidin-4(1H)-one (259 mg, 0.941 mmol) in THF (10 mL) at −78° C. was added dropwise 1.6 M n-butyllithium in hexane (1.29 mL, 2.07 mmol). After 20 min, DMF (0.146 mL, 1.88 mmol) was added, and the mixture was allowed to −30° C. for 30 min. The mixture was poured into water (50 mL) and brine (50 mL). Extraction with EtOAc (100 mL), washing with brine, drying over MgSO4, filtration and concentration under reduced pressure gave the title compound (205 mg, 97%) as yellow solid:

WORKUP

后处理

  1. waitthe mixture was allowed to −30° C. for 30 min
  2. extractionExtraction with EtOAc (100 mL)
  3. washwashing with brine
  4. dry with materialdrying over MgSO4, filtration and concentration under reduced pressure