반응 #83764

ord-63b91ed0e8e4469f9996a933e45c1c30

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타A procedure similar to that described in Preparation 15

실험 절차

A procedure similar to that described in Preparation 15 was repeated, except that 45 g of 2-hydroxymethyl-1H-imidazo[4,5-b]pyridine, 13.17 g of sodium hydride (as a 55% by weight dispersion in mineral oil), 20.7 ml of methyl iodide and 1.43 liter of dimethylformamide were used, to give the title compound as a crude product. This crude product was purified by column chromatography through silica gel, using a gradient elution method, with mixtures of ethyl acetate and methanol in ratios ranging from 1:0 to 1:1 by volume as the eluent, to give 3.24 g of the title compound, melting at 130°-132° C.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05624935uspto-grants-1997_04