HRID1660752

反应详情

EQUATION

反应方程式

HRID 1660752 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Add n-butyl lithium (2.5 M in hexanes, 174 mL, 0.43 mmol) to a stirred solution of 7-(1-ethyl-propyl)-3-(2-methoxymethyl-thiazol-5-yl)-2,5-dimethyl-pyrazolo[1,5-a]pyrimidine (150 mg, 0.43 mmol) in THF (3 mL) at −78° C. Stir for 30 min and add N-chlorosuccinimide (87 mg, 0.653 mmol). Stir 30 min and then warm the reaction slowly to room temperature allowing the reaction to continue overnight. Quench the reaction by adding saturated ammonium chloride solution, extract with ethyl acetate, dry over sodium sulfate, filter, and concentrate to a residue. Purify by flash chromatography, eluting with hexanes/ethyl acetate (10/2) to give the title compound (7 mg). MS (APCI) m/z (35Cl) 379.3 (M+1)+.

WORKUP

后处理

  1. stirringStir 30 min
  2. temperaturewarm
  3. customthe reaction slowly to room temperature
  4. customthe reaction
  5. waitto continue overnight
  6. customQuench
  7. customthe reaction
  8. extractionextract with ethyl acetate
  9. dry with materialdry over sodium sulfate
  10. filtrationfilter
  11. concentrationconcentrate to a residue
  12. customPurify by flash chromatography
  13. washeluting with hexanes/ethyl acetate (10/2)