HRID2189819

反应详情

EQUATION

反应方程式

HRID 2189819 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

A solution of ethyl 3-[4-(5-{3-cyano-4-[(1-methylethyl)oxy]phenyl}-1,2,4-oxadiazol-3-yl)-1H-indazol-1-yl]-2,2-dimethylpropanoate (D109) (100 mg, 0.21 mmol) in ethanol (2 ml) was treated with 2M sodium hydroxide aqueous solution (1 ml, large excess) and heated at 80° C. for 2 hours. The reaction mixture was cooled and most the ethanol was removed in vacuo. The residue was diluted with water (3 ml) and acidified with a concentrated.HCl aqueous solution and extracted with EtOAc (3×10 ml). The combined extracts were dried and concentrated in vacuo. Purification of the residue by MDAP gave the desired product (5 mg, 5%) as a colourless solid. MS (ES) C24H23N5O4 requires 445; found (MH+) 446.

WORKUP

后处理

  1. temperatureThe reaction mixture was cooled
  2. custommost the ethanol was removed in vacuo
  3. additionThe residue was diluted with water (3 ml)
  4. extractionHCl aqueous solution and extracted with EtOAc (3×10 ml)
  5. customThe combined extracts were dried
  6. concentrationconcentrated in vacuo
  7. customPurification of the residue by MDAP