HRID522683

反应详情

EQUATION

反应方程式

HRID 522683 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

5

PROCEDURE

实验过程

To a mixture of tert-butyl 4-(5-benzyl-4-(trifluoromethylsulfonyloxy)pyrimidin-2-yl)piperazine-1-carboxylate (280 mg, 0.56 mmol) and iron (III) acetylacetonate (21 mg, 0.06 mmol) in THF (5 mL, dry) and 1-methyl-2-pyrrolidinone (1 mL) was added methylmagnesium chloride (1.68 mL, 1.68 mmol). The reaction mixture was stirred at RT for 1 h, and diluted with ethyl acetate (100 mL) and sat. aq. NH4Cl (100 mL). The organic layer was washed with brine (100 mL), dried over sodium sulfate, filtered and evaporated to give tert-butyl 4-(5-benzyl-4-methylpyrimidin-2-yl)piperazine-1-carboxylate (crude, 250 mg) as a yellow solid. MS (ES+) C21H28N4O2 requires: 368, found: 369 [M+H]+.

WORKUP

后处理

  1. washThe organic layer was washed with brine (100 mL)
  2. dry with materialdried over sodium sulfate
  3. filtrationfiltered
  4. customevaporated