HRID2199513

反应详情

EQUATION

反应方程式

HRID 2199513 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. customthe ice bath was removed
  2. stirringthe mixture was stirred for a further 3 minutes at room temperature
  3. customThe suspension formed
  4. stirringThe mixture was stirred for 4 hours at 40° C.
  5. extractionThe mixture was extracted with acetic ester (2×)
  6. dry with materialThe combined organic phases were dried (Na2SO4)
  7. filtrationfiltered
  8. concentrationconcentrated by evaporation
  9. customThe resulting residue was purified by means of chromatography (hexane/acetic ester 4:1) (yield: 41%)