反应 #1702166

ord-ab74b4e473ee41589888264be644125d

反应方程式

CC(C)(C)OC(=O)Nc1cncc(CCc2cc(CNc3nc(Cl)ncc3Cl)ccc2NC(=O)OC(C)(C)C)c1
tert-butyl {5-[2-(2-[(tert-butoxycarbonyl)amino]-5-{[(2,5-dichloropyrimidin-4-yl)amino]methyl}phenyl)ethyl]pyridin-3-yl}carbamate
CO
methanol
Cl
hydrogen chloride
Cl.Cl.Cl.Nc1cncc(CCc2cc(CNc3nc(Cl)ncc3Cl)ccc2N)c1
desired product
收率 98.0%
Cl.Cl.Cl.Nc1cncc(CCc2cc(CNc3nc(Cl)ncc3Cl)ccc2N)c1
N-{4-Amino-3-[2-(5-aminopyridin-3-yl)ethyl]benzyl}-2,5-dichloropyrimidin-4-amine trihydrochloride
收率 98.0%

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    浓缩concentrated under vacuum

实验过程

Into a reaction flask were added tert-butyl {5-[2-(2-[(tert-butoxycarbonyl)amino]-5-{[(2,5-dichloropyrimidin-4-yl)amino]methyl}phenyl)ethyl]pyridin-3-yl}carbamate (0.44 g, 0.75 mmol), methanol (3 mL), and a solution of hydrogen chloride in 1,4-dioxane (5 mL, 4.0 M). The reaction mixture was stirred at rt overnight and concentrated under vacuum to give the desired product as a white powder (0.40 g, 98%). LCMS for C18H19Cl2N6 (M+H)+: m/z=389.0, 391.0.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US08765727B2uspto-grants-2014_07