HRID714850

反应详情

EQUATION

反应方程式

HRID 714850 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of (3S)-1-(2-chloropyrimidin-4-yl)-3-cyclopropyl-2-oxopyrrolidine-3-carbonitrile (130 mg) obtained in Step E of Example 103, 2-(4-amino-1H-pyrazol-1-yl)-N-methylacetamide (84 mg) and acetic acid (31 μL) in ethanol (3.0 mL) was stirred in a microwave reactor at 150° C. for 1 hr, and the solvent was evaporated under reduced pressure. The obtained residue was purified by silica gel column chromatography (hexane/ethyl acetate). To a solution of the residue (190 mg) in ethanol (5.0 mL) was added 1 M hydrochloric acid (0.50 mL), and the solvent was evaporated under reduced pressure. The residue was recrystallized (diisopropyl ether/ethanol) to give the title compound (120 mg).

WORKUP

后处理

  1. customthe solvent was evaporated under reduced pressure
  2. customThe obtained residue was purified by silica gel column chromatography (hexane/ethyl acetate)
  3. additionTo a solution of the residue (190 mg) in ethanol (5.0 mL) was added 1 M hydrochloric acid (0.50 mL)
  4. customthe solvent was evaporated under reduced pressure
  5. customThe residue was recrystallized (diisopropyl ether/ethanol)