반응 #1563899

ord-5e17b9c89f1840d683aa9a042fb62ec8

반응 방정식

Nc1nccc2c1nc(Sc1cc3c(cc1Br)OCO3)n2CCCO
Compound 0403-51
Nc1nccc2c1nc(Sc1cc3c(cc1Br)OCO3)n2CCCO
3-(4-Amino-2-(6-bromobenzo[d][1,3]dioxol-5-ylthio)-1H-imidazo[4,5-c]pyridin-1-yl)propan-1-ol
CCN(CC)CC
NEt3
CS(=O)(=O)Cl
MsCl
CS(=O)(=O)OCCCn1c(Sc2cc3c(cc2Br)OCO3)nc2c(N)nccc21
title compound 0404-51
CS(=O)(=O)OCCCn1c(Sc2cc3c(cc2Br)OCO3)nc2c(N)nccc21
3-(4-Amino-2-(6-bromobenzo[d][1,3]dioxol-5-ylthio)-1H-imidazo[4,5-c]pyridin-1-yl)propyl methanesulfonate

용매

반응 조건

온도
40°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    농축The mixture was concentrated
  2. 2
    기타purified by column chromatography on silica gel (CH2Cl2/MeOH=50/1)

실험 절차

Compound 0403-51 (264 mg, 0.624 mmol) was dissolved in hot anhydrous dioxane (8.6 mL). The solution was cooled to 40° C. and was treated with NEt3 (189 mg, 1.87 mmol) and MsCl (107 mg, 0.935 mmol) for 20 min. The mixture was concentrated and purified by column chromatography on silica gel (CH2Cl2/MeOH=50/1) to give the title compound 0404-51 as a white solid (143 g, 50%): LCMS: 501 [M+1]+.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US09402832B2uspto-grants-2016_08