HRID1429632

反应详情

EQUATION

反应方程式

HRID 1429632 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Trifluoroacetic acid (1 mL) was added to a solution of t-butyl 5-difluoromethylpyrazine-2-carboxylate (175 mg) in dichloromethane (1 mL), and the mixture was stirred at RT for 5 h. Ether and 5 N NaOH were added to the reaction solution. The aqueous layer was separated and made acidic with 5 N hydrochloric acid. EtOAc was added to the aqueous layer, and the organic layer was separated. The organic layer was dried over anhydrous MgSO4, and the insoluble matter was separated by filtration. The filtrate was concentrated to obtain the title compound (100 mg). 1H-NMR (CDCl3) δ (ppm): 6.80 (t, J=54.4 Hz, 1H), 9.02 (s, 1H), 9.47 (s, 1H).

WORKUP

后处理

  1. customThe aqueous layer was separated
  2. additionEtOAc was added to the aqueous layer
  3. customthe organic layer was separated
  4. dry with materialThe organic layer was dried over anhydrous MgSO4
  5. customthe insoluble matter was separated by filtration
  6. concentrationThe filtrate was concentrated