HRID2199513
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
(2R,3R)-3-Benzyloxybutan-2-ol in diethyl ether were admixed with sodium hydride in portions at 0° C. with stirring. After 10 minutes, the ice bath was removed and the mixture was stirred for a further 3 minutes at room temperature. The suspension formed was added, at 0° C., to a solution of 2,4-dichloro-5-iodopyrimidine. The mixture was stirred for 4 hours at 40° C. and then admixed with dilute sodium chloride solution. The mixture was extracted with acetic ester (2×). The combined organic phases were dried (Na2SO4), filtered and concentrated by evaporation. The resulting residue was purified by means of chromatography (hexane/acetic ester 4:1) (yield: 41%).
WORKUP
后处理
- customthe ice bath was removed
- stirringthe mixture was stirred for a further 3 minutes at room temperature
- customThe suspension formed
- stirringThe mixture was stirred for 4 hours at 40° C.
- extractionThe mixture was extracted with acetic ester (2×)
- dry with materialThe combined organic phases were dried (Na2SO4)
- filtrationfiltered
- concentrationconcentrated by evaporation
- customThe resulting residue was purified by means of chromatography (hexane/acetic ester 4:1) (yield: 41%)