HRID1052103

反应详情

EQUATION

反应方程式

HRID 1052103 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
70 °C

PROCEDURE

实验过程

To methyl 2-(3-acetyl-5-hydroxy-1H-indazol-1-yl)acetate (1.80 g, 7.25 mmol) in CH3CN (75 mL) was added 2-(chloromethyl)pyrimidine hydrochloride (1.32 g, 7.98 mmol) and Cs2CO3 (5.91 g, 18.13 mmol). The reaction mixture was stirred at 70° C. for 2 h. The reaction mixture was filtered and washed with CH3CN. The solvent was removed under reduced pressure and the crude residue was purified by flash column chromatography on silica gel (c-hexane/EtOAc 1:1 to 1:3). TLC, Rf (c-hexane/EtOAc 1:3)=0.35; MS (LC/MS): 340.9 [M+H]+, 363.0 [M+Na]+; tR (HPLC conditions e): 3.64 min.

WORKUP

后处理

  1. filtrationThe reaction mixture was filtered
  2. washwashed with CH3CN
  3. customThe solvent was removed under reduced pressure
  4. customthe crude residue was purified by flash column chromatography on silica gel (c-hexane/EtOAc 1:1 to 1:3)
  5. custom3.64 min.