반응 #53430

ord-d11bec94770c4b5c9e1b124727c52863

반응 조건

온도
25°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    여과the precipitated urea is filtered off with suction
  2. 2
    세척the organic phase is washed twice each with 500 ml of 2 M hydrochloric acid and water
  3. 3
    농축The organic phase is concentrated
  4. 4
    workup.DISTILLATIONdistilled

실험 절차

450 g (3 mol) of 4-methylphenyl-acetic acid (Aldrich), 1.13 l (12 mol) of tert-butanol and 90 g (0.74 mol) of 4-(N,N-dimethylamino)pyridine are dissolved in 2 l of dichloromethane. After addition of 680 g (3.3 mol of dicyclohexylcarbodiimide, dissolved in 400 ml of dichloromethane, the mixture is stirred at 25° C. for 20 h, the precipitated urea is filtered off with suction and flashed with 200 ml of dichloromethane, and the organic phase is washed twice each with 500 ml of 2 M hydrochloric acid and water. The organic phase is concentrated and distilled.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US06858622B2uspto-grants-2005_02