HRID1769209

反应详情

EQUATION

反应方程式

HRID 1769209 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 1-[2-(t-butoxycarbonylamino)pyridin-3-yl]hexan-2-one (42) (4.2 g) (prepared, e.g, as described in Preparation 29), in dichloromethane (25 ml) and trifluoroacetic acid (10 ml) was stirred at room temperature overnight. The solution was concentrated under vacuum and the residue was partitioned between aqueous ammonium hydroxide and ether. The ether layer was washed with brine, dried, and the solvent was evaporated. The residue was further purified by silica gel chromatography, eluting with 30% ethyl acetate-hexane, to give 2-(n-butyl)-7-azaindole (2.9 g), a compound of Formula (43), as an oil, which crystallized on standing to a solid, m.p. 46°-47° C.

WORKUP

后处理

  1. concentrationThe solution was concentrated under vacuum
  2. customthe residue was partitioned between aqueous ammonium hydroxide and ether
  3. washThe ether layer was washed with brine
  4. customdried
  5. customthe solvent was evaporated
  6. customThe residue was further purified by silica gel chromatography
  7. washeluting with 30% ethyl acetate-hexane