反応 #60824

ord-d48c83fc7ad5411db027175bd48b26b8

反応方程式

CC(C)OC(=O)N=NC(=O)OC(C)C
Diisopropyl azodicarboxylate
Cn1cnc(-c2ccccc2)c1-c1nc2c(N)ncnc2[nH]1
8-(1-methyl-4-phenyl-1H-imidazol-5-yl)-9H-purin-6-amine
Cn1cnc(-c2ccccc2)c1-c1nc2c(N)ncnc2[nH]1
8-(1-Methyl-4-phenyl-1H-imidazol-5-yl)-9H-purin-6-amine
OC1CCCCC1
cyclohexanol
c1ccc(P(c2ccccc2)c2ccccc2)cc1
triphenylphosphine
Cn1cnc(-c2ccccc2)c1-c1nc2c(N)ncnc2n1C1CCCCC1
title compound
収率 11.0%
Cn1cnc(-c2ccccc2)c1-c1nc2c(N)ncnc2n1C1CCCCC1
9-Cyclohexyl-8-(1-methyl-4-phenyl-1H-imidazol-5-yl)-9H-purin-6-amine
収率 11.0%

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度was heated at 40° C. for 48 hours
  2. 2
    workup.WAITat 55° C. for 24 hours
  3. 3
    その他The solvent was then evaporated in vacuo
  4. 4
    その他to give a brown oil
  5. 5
    その他Purification by preparative LCMS

実験手順

Diisopropyl azodicarboxylate (0.1 mL) was added to a solution of 8-(1-methyl-4-phenyl-1H-imidazol-5-yl)-9H-purin-6-amine (Example 3) (75 mg), cyclohexanol (0.07 mL) and triphenylphosphine (0.14 g) in THF (4 mL) under an inert atmosphere. After stirring at ambient temperature for 48 hours the reaction mixture was heated at 40° C. for 48 hours and then at 55° C. for 24 hours. The solvent was then evaporated in vacuo to give a brown oil. Purification by preparative LCMS gave the title compound as a white solid (11 mg, 11%);

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07427616B2uspto-grants-2008_09