HRID2204272

反应详情

EQUATION

反应方程式

HRID 2204272 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

To a solution of (1H-benzo[d]imidazol-4-yl)(1-methyl-1H-spiro[chromeno[4,3-c]pyrazole-4,4′-piperidine]-1′-yl)methanone (21 mg, 0.052 mmol) in dry THF (0.2 mL) under N2 was added NaH (1.9 mg, 0.079 mmol) at 0° C. After 30 min, MeI (3.3 μL, 0.052 mmol) was added and the mixture was stirred at 0° C. for 1 h. The reaction mixture was quenched with water and the solvent removed under vacuum to yield a crude residue that was taken up in methanol and purified by reverse phase HPLC to give (3-methylbenzoimidazol-4-yl)-(1-methyl-1H-Spiro[chromeno[4,3-c]pyrazole-4,4′-piperidine]-1′-yl)methanone. ESI-MS m/z talc. 413.5, found 414.5 (M+1)+. Retention time: 1.13 minutes (3 min run).

WORKUP

后处理

  1. customThe reaction mixture was quenched with water
  2. customthe solvent removed under vacuum
  3. customto yield a crude residue that
  4. custompurified by reverse phase HPLC