HRID2169141

反应详情

EQUATION

反应方程式

HRID 2169141 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a stirred solution of 5-benzyloxy-2-biphenyl-2-ylmethyl-6-hydroxypyrimidine-4-carboxylic acid (2-hydroxyethyl)-methyl-amide (10-01) (400 mg, 0.853 mmol) in dichloromethane (10 mL) was added triphenyl phosphine (336.46 mg, 1.27 mmol) at room temperature. The mixture was stirred for 10 min. Then diisopropyl azodicarboxylate (diisopropylazodicarboxylate) (258.4 mg, 1.27 mmol) was added at room temperature and the resultant mixture was stirred for another 2 h. After completion of the reaction, the mixture was concentrated under reduced pressure to get a crude product, which was purified using normal silica column using 2% methanol in dichloromethane to of ford 9-benzyloxy-6-biphenyl-2-ylmethyl-2-methyl-3,4-dihydro-2H-pyrazino[1,2-c]pyrimidine-1,8-dione (11-01) (200 mg, 51.94%) as a white solid.

WORKUP

后处理

  1. customAfter completion of the reaction
  2. concentrationthe mixture was concentrated under reduced pressure