반응 #60790

ord-c19045a302f14666847a11bd7e283cf0

반응 방정식

O=P(O)(O)O
phosphoric acid
O=P12OP3(=O)OP(=O)(O1)OP(=O)(O2)O3
Phosphorous pentoxide
Cn1cnc(-c2ccccc2)c1C(=O)Nc1c(N)ncnc1N
N-(4,6diaminopyrimidin-5-yl)-1-methyl-4-phenyl-1H-imidazole-5-carboxamide
Cn1cnc(-c2ccccc2)c1C(=O)Nc1c(N)ncnc1N
intermediate 7
Cn1cnc(-c2ccccc2)c1C(=O)Nc1c(N)ncnc1N
N-(4,6diaminopyrimidin-5-yl)-1-methyl-4-phenyl-1H-imidazole-5-carboxamide
N
NH3
Cn1cnc(-c2ccccc2)c1-c1nc2c(N)ncnc2[nH]1
title compound
수율 96.9%
Cn1cnc(-c2ccccc2)c1-c1nc2c(N)ncnc2[nH]1
8-(1-Methyl-4-phenyl-1H-imidazol-5-yl)-9H-purin-6-amine
수율 96.9%

반응 조건

온도
160°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.ADDITIONIce was added to the cooled mixture, which
  2. 2
    여과the resultant precipitate filtered off
  3. 3
    세척washed with water
  4. 4
    기타dried at 60° C. in vacuo

실험 절차

Phosphorous pentoxide (1.06 g) was added to N-(4,6diaminopyrimidin-5-yl)-1-methyl-4-phenyl-1H-imidazole-5-carboxamide (intermediate 7) (171 mg) followed by phosphoric acid (85%, 0.76 mL) and heated at 160° C. for 72 hours. Ice was added to the cooled mixture, which was then adjusted to pH 5 with aqueous NH3, the resultant precipitate filtered off, washed with water and dried at 60° C. in vacuo to give the title compound as a cream solid (156 mg, 89%);

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07427616B2uspto-grants-2008_09