تفاعل #730680

ord-f062be62da8d4b0fb702aa3c060dae3c

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    ترشيحis filtered through an EXTUBE extraction column with EtOAc (200 ml)
  2. 2
    أخرىThe filtrate is evaporated
  3. 3
    أخرىthe resulting crude product is purified on silica (90 g) with cyclohexane/EtOAc 95:5 to 70:30

الإجراء التجريبي

A mixture of (4-bromo-benzyl)-carbamic acid tert-butyl ester (600 mg), 3-hydroxybenzeneboronic acid (373 mg), sodium carbonate (333 mg), palladium (II) acetate (10 mg) and tricyclohexylphosphine (13 mg) in water (3.5 ml) and dioxane (14 ml) is kept at 90° C. under micro wave conditions for 230 min. The mixture is cooled down to rt and is filtered through an EXTUBE extraction column with EtOAc (200 ml). The filtrate is evaporated and the resulting crude product is purified on silica (90 g) with cyclohexane/EtOAc 95:5 to 70:30 to afford pure (3′-hydroxy-biphenyl-4-ylmethyl)-carbamic acid tert-butyl ester.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07700605B2uspto-grants-2010_04