HRID1031762

反应详情

EQUATION

反应方程式

HRID 1031762 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 1H-indazole-3-acetic acid (1.0 g) prepared according to J. Am. Chem. Soc., 79, 5245 (1957), in methanol (30 ml) containing five drops of concentrated sulfuric acid was refluxed for 8 hours. The reaction mixture was then concentrated to a low volume and diluted with ethyl acetate (20 ml). The organic layer was washed with water (2×10 ml) and then with sodium bicarbonate solution (10 ml, 10%). The ethyl acetate layer was collected and then dried to obtain the title compound (yield: 0.8g; m.p. 146° C.).

WORKUP

后处理

  1. temperaturewas refluxed for 8 hours
  2. concentrationThe reaction mixture was then concentrated to a low volume
  3. additiondiluted with ethyl acetate (20 ml)
  4. washThe organic layer was washed with water (2×10 ml)
  5. customThe ethyl acetate layer was collected
  6. customdried