HRID450833

反应详情

EQUATION

反应方程式

HRID 450833 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
90 °C

PROCEDURE

实验过程

Methyl 2-chloro-5,6,7,8,9,10-hexahydrocyclohepta[b]indole-6-carboxylate (10 g, 36 mmol) was dissolved in 7 N ammonia in methanol (350 mL) and transferred to Parr pressure reactor. The reaction vessel was purged briefly to displace any air with Nitrogen. The reaction was then heated to 90° C. for 48 h. The reaction was cooled to r.t. and the solvent removed in vacuo, the crude residue was applied to a Biotage and eluted with grading (1/1 heptane/ethyl acetate to 0/1 heptane/ethyl acetate) to afford product as an off white foam, which was triturated with DCM to afford pure product 2 g (21%) as an off white solid.

WORKUP

后处理

  1. customThe reaction vessel was purged briefly
  2. temperatureThe reaction was cooled to r.t.
  3. customthe solvent removed in vacuo
  4. washeluted with grading (1/1 heptane/ethyl acetate to 0/1 heptane/ethyl acetate)
  5. customto afford product as an off white foam, which
  6. customwas triturated with DCM