HRID1290665

反应详情

EQUATION

反应方程式

HRID 1290665 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To 2-methylthio-4-benzylamino-5-nitro-6-(2-benzyloxy-5-cyanophenoxy)pyrimidine (1.82 g, 3.76 mmol) in 40 mL MeOH and 40 mL dioxane at 0° C. was added potassium metabisulfite (KHSO5) (3.59 g, 11.3 mmol) in 40 mL water. The suspension was allowed to warm to ambient temperature and stirred for 15 hours. The reaction was concentrated to 25 mL and extracted with methylene chloride (200 mL). The organic layer was dried (Na2 SO4), evaporated and chromatographed on silica gel (2:1, hexane/ethyl acetate) to afford 0.26 g of 2-methylsulfonyl-4-benzylamino-5-nitro-6-(2-benzyloxy-5-cyanophenoxy)pyrimidine, a compound of formula (F), as a white solid.

WORKUP

后处理

  1. concentrationThe reaction was concentrated to 25 mL
  2. extractionextracted with methylene chloride (200 mL)
  3. customThe organic layer was dried (Na2 SO4)
  4. customevaporated
  5. customchromatographed on silica gel (2:1, hexane/ethyl acetate)