HRID2307852

反应详情

EQUATION

反应方程式

HRID 2307852 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
40 °C

PROCEDURE

实验过程

A sodium methoxide solution, which had been prepared from 190 mg (8.26 mmol) of NaOMe and 30 ml of abs. methanol, was added to a solution of 20.0 g (97.7 mmol) of 1-(2-fluorobenzyl)-3-cyanoindazole (from Example IX) in 200 ml of methanol, and the mixture was stirred at 40° C. for 22 h. After addition of 0.46 ml of acetic acid and 4.30 g of NH4Cl, the mixture was stirred at 40° C. for another 24 h and subsequently concentrated to dryness using a rotary evaporator. The residue was taken up in acetone and the remaining precipitate was filtered off with suction, giving, after drying under high vacuum, the product in the form of a light-beige powder.

WORKUP

后处理

  1. stirringthe mixture was stirred at 40° C. for another 24 h
  2. concentrationsubsequently concentrated to dryness
  3. customa rotary evaporator
  4. filtrationthe remaining precipitate was filtered off with suction
  5. customgiving
  6. customafter drying under high vacuum