HRID2189796

反应详情

EQUATION

反应方程式

HRID 2189796 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Ethyl 3-(4-cyano-1H-indazol-1-yl)-2,2-dimethylpropanoate (D102) (348 mg, 1.28 mmol), hydroxylamine hydrochloride (1.087 g, 10.26 mmol), NaHCO3 (1.078 g, 12.83 mmol) in MeOH (20 ml) was heated at 65° C. for 24 h then at room temperature over the weekend. The mixture was filtered, concentrated, treated with water and vigorously stirred for 10 mins, filtered and dried to give a colourless solid, dried overnight in vacuo at 45° C. to give the title compound (373 mg, 90%). MS (ES) C15H20N4O3 requires 304, found 305 [M+H]+

WORKUP

后处理

  1. customat room temperature
  2. filtrationThe mixture was filtered
  3. concentrationconcentrated
  4. additiontreated with water
  5. filtrationfiltered
  6. customdried
  7. customto give a colourless solid
  8. customdried overnight in vacuo at 45° C.