反応 #1563899

ord-5e17b9c89f1840d683aa9a042fb62ec8

反応方程式

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

溶媒

反応条件

温度
40°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    濃縮The mixture was concentrated
  2. 2
    その他purified by column chromatography on silica gel (CH2Cl2/MeOH=50/1)

実験手順

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]+.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US09402832B2uspto-grants-2016_08