反応 #52156

ord-f365d521b5b54e1493008a822705eacd

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度The reaction mixture was refluxed under nitrogen for ˜1 hr
  2. 2
    濃縮The reaction mixture was then concentrated in vacuo
  3. 3
    その他azeotroped with toluene (1×5 mL)

実験手順

N-(3,5-Dichlorobenzenesulfonyl)-octahydroisoindole-1-carboxylic acid (1 gm, 2.64 mmol) was dissolved in CH2Cl2 (5 mL) containing DMF (1 drop) and SOCl2 (770 μL, 10.56 mmol). The reaction mixture was refluxed under nitrogen for ˜1 hr. The reaction mixture was monitored by TLC for the formation of the acid chloride. The reaction mixture was then concentrated in vacuo and azeotroped with toluene (1×5 mL) to afford N-(3,5-dichlorobenzenesulfonyl)-octahydroisoindole-1-carboxylic acid chloride which was used without further purification in the subsequent step.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US06855708B2uspto-grants-2005_02