HRID2099765

反应详情

EQUATION

反应方程式

HRID 2099765 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of (±)-2-(1-(6-bromopyridin-2-yl)-2-(7-methyl-2-((2-(trimethylsilyl)ethoxy)methyl)-2H-indazol-5-yl)ethyl)isoindoline-1,3-dione (1 mmol) in methanol (10 mL) was treated with hydrazine (0.16 mL, 5 mmol) at room temperature for 30 min and at 70° C. for 5 h. The mixture was concentrated in vacuo and the residue was partitioned between 1N sodium hydroxide and ethyl acetate. The organic layer was washed with water, brine, dried and concentrated. The pale yellow oil (100%) was pure enough to carry on. MS (ESI) [M+H]+=461. HPLC tR=1.62 min.

WORKUP

后处理

  1. concentrationThe mixture was concentrated in vacuo
  2. customthe residue was partitioned between 1N sodium hydroxide and ethyl acetate
  3. washThe organic layer was washed with water, brine
  4. customdried
  5. concentrationconcentrated