HRID248927
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
A solution of 1-[2-(t-butoxycarbonylamino)pyridin-3-yl]hexan-2-one (Y) (4.2 g) (prepared, e.g, as described in Preparation 18), 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 (AB), as an oil, which crystallized on standing to a solid, m.p. 46°-47° C.
WORKUP
后处理
- concentrationThe solution was concentrated under vacuum
- customthe residue was partitioned between aqueous ammonium hydroxide and ether
- washThe ether layer was washed with brine
- customdried
- customthe solvent was evaporated
- customThe residue was further purified by silica gel chromatography
- washeluting with 30% ethyl acetate-hexane