반응 #705933

ord-333894c2be5f45d6b900a7e043f1db3f

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    세척The reaction solution is washed with 150 ml of water and 150 ml of brine
  2. 2
    농축concentrated in vacuo to a volume of 50 ml
  3. 3
    기타chromatographed on silica gel 60 (40-63 μm)

실험 절차

5.89 g of triethylamine, 8.14 g of triphenylchloromethane and 0.10 g of 4-N,N-dimethylaminopyridine are added in succession to a suspension of 10.37 g of 3-bromo-2-[2'-(1H-tetrazol-5-yl)-phenyl]-5-methylbenzofuran in 300 ml of CH2Cl2 and the batch is stirred for 3 hours at room temperature. The reaction solution is washed with 150 ml of water and 150 ml of brine, concentrated in vacuo to a volume of 50 ml and chromatographed on silica gel 60 (40-63 μm) using CH2Cl2 as eluant. The product, of Rf =0.82 (CH2Cl2 /CH3OH (95:5)), yields crystalline 3-bromo-2-[2-(1-trityltetrazol-5-yl)-phenyl]-5-methylbenzofuran, m.p. 199-200°, from ether.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05955487uspto-grants-1999_09