反応 #1095472

ord-b1564b975d7f4beab8168da06767de58

反応条件

温度
110°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    ろ過filtered through Celite
  2. 2
    洗浄washed with brine
  3. 3
    乾燥dried (Na2SO4)
  4. 4
    その他purified by silica gel chromatography

実験手順

To a solution of (2S,3R)-3-(n-butyl)-2-hydroxysuccinic acid F-4 (300 mg, 1.58 mmol) and powdered molecular sieves (1 g) in trimethyl orthobenzoate (5 mL) and toluene (5 ml) was added 10-Camphorsulfonic acid (20 mg) and the reaction was heated at 110° C. under vacuum (20 torr) for 5 h. The solution was diluted with ethyl acetate, filtered through Celite and washed with brine, dried (Na2SO4) and then purified by silica gel chromatography to afford 1.2 mmol 2-(2-methoxy-2-phenyl-4-oxo-1,3-dioxolan-5-yl)hexanoic acid I-1 (40%).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US06797820B2uspto-grants-2004_09