HRID1290665
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- concentrationThe reaction was concentrated to 25 mL
- extractionextracted with methylene chloride (200 mL)
- customThe organic layer was dried (Na2 SO4)
- customevaporated
- customchromatographed on silica gel (2:1, hexane/ethyl acetate)