反応 #93584

ord-7dad1f2413ae4720a170013ffa19b5ad

反応条件

温度
15°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度the resulting mixture warmed to 80°-90° C. for one hour
  2. 2
    抽出extracted with CH2Cl2, and vacuum
  3. 3
    workup.DISTILLATIONdistilled

実験手順

A solution of 2-(3,4-dimethoxyphenyl)-2-isopropylacetonitrile (6a) in toluene is slowly added to sodium amide (1.5 eq) in toluene, and the resulting mixture warmed to 80°-90° C. for one hour. The mixture was then cooled to 15° C. and 1-bromo-3-chloropropane (2 eq) slowly added and stirred for two hours at room temperature. The mixture is then carefully poured into ice water, extracted with CH2Cl2, and vacuum distilled to yield 2-(3,4-dimethoxyphenyl)-2-isopropyl-2-(3-chloropropyl)acetonitrile (21, b.p. 160°-165°/0.05 mmHg).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US04613606uspto-grants-1986_09