HRID2105269

反应详情

EQUATION

反应方程式

HRID 2105269 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

n-BuLi 2.0M (ALDRICH, 0.18 ml) was added dropwise, with vigorous stirring, to a solution of 5-bromo-2-(4-trifluoromethylphenyl)pyrimidine (60 mg) in THF (2 ml) at −78° C. After stirring for 1 hour, tributyltin chloride (97 μl) was added dropwise at −78° C., under argon atmosphere. After 1 hour 30 minutes at −78° C., the reaction was quenched with 1 N NH4Cl (5 ml), diluted, extracted with ethyl acetate (3×10 ml), washed with brine, dried over MgSO4, concentrated under vacuum and purified by chromatography column using CH2Cl2-hexane 1:8 as eluent to give 75 mg of the desired product as a colorless oil.

WORKUP

后处理

  1. waitAfter 1 hour 30 minutes at −78° C.
  2. customthe reaction was quenched with 1 N NH4Cl (5 ml)
  3. additiondiluted
  4. extractionextracted with ethyl acetate (3×10 ml)
  5. washwashed with brine
  6. dry with materialdried over MgSO4
  7. concentrationconcentrated under vacuum
  8. custompurified by chromatography column