HRID38519

反应详情

EQUATION

反应方程式

HRID 38519 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

tert-Butyl 4-chloro-5,8-dihydropyrido[4′,3′:4,5]thieno[2,3-d]pyrimidine-7(6H)-carboxylate from Example 11A (500 mg, 1.54 mmol) was dissolved in 2-methoxyethanol (5 mL), and (R)-methylbenzylamine (223 mg, 1.84 mmol) and triethylamine (621 mg, 6.14 mmol) were added. The mixture was heated to 100° C. for 2 h, then diluted with ethyl acetate and washed with water. The organic layer was dried over sodium sulfate, and the solvent was removed in vacuo. The crude product was purified by column chromatography on silica gel (eluent: cyclohexane/ethyl acetate 3:1) to yield 474 mg (75%) of the title compound.

WORKUP

后处理

  1. washwashed with water
  2. dry with materialThe organic layer was dried over sodium sulfate
  3. customthe solvent was removed in vacuo
  4. customThe crude product was purified by column chromatography on silica gel (eluent: cyclohexane/ethyl acetate 3:1)