HRID1412040

反应详情

EQUATION

反应方程式

HRID 1412040 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a stirred solution of MeNH2 (30% wt in water) (2.5 g, 20 mmol) in acetone (10 mL) at 0° C. (ice bath) was added K2CO3 (415 mg, 3 mmol), followed by the dropwise addition of a solution of 5-(bromomethyl)-1-methyl-3-nitro-1H-pyrazole (220 mg, 1 mmol) in acetone (5 mL). The reaction mixture was then warmed to room temperature and stirred for 3 h. The solvent was removed and the residue was extracted with methylene chloride (3×15 mL), dried over Na2SO4 and concentrated to afford 302a as a yellow oil (170 mg, 99%), which was used in the next step without additional purification. LCMS: (M+H)+ 171

WORKUP

后处理

  1. customThe solvent was removed
  2. extractionthe residue was extracted with methylene chloride (3×15 mL)
  3. dry with materialdried over Na2SO4
  4. concentrationconcentrated