反応 #71489

ord-7fb62231dfe84621899ce1be9659ae2b

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    抽出extracted with Et2O
  2. 2
    workup.ADDITIONThe aqueous layer was acidified to pH 4 by addition of a 2 N aqueous solution of HCl
  3. 3
    ろ過The resulting white precipitate was collected by vacuum filtration

実験手順

A mixture of 5-(2-chloro-6-fluoro-3,5-dimethoxy-phenyl)-quinoline-8-carboxylic acid ethyl ester (Step 176.2) (235 mg, 0.60 mmol), a 2 N aqueous solution of LiOH (3 mL) and THF (3 mL) was stirred for 20 h at rt, diluted with H2O and extracted with Et2O. The aqueous layer was acidified to pH 4 by addition of a 2 N aqueous solution of HCl. The resulting white precipitate was collected by vacuum filtration providing 210 mg of the title compound: ESI-MS: 362.1 [M+H]+; tR=4.24 min (System 1).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08536175B2uspto-grants-2013_09