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Cyclohexanol → 9-Cyclohexyl-8-(1-methyl-4-phenyl-1H-imidazol-5-yl)-9H-purin-6-amine

HRID 32546
ノート
印刷プレビュー

反応式

HRID 32546 の反応式
N(C(OC(C)C)=O)=NC(OC(C)C)=O.[CH3:15][N:16]1[C:20]([C:21]2[NH:22][C:23]3[C:28]([N:29]=2)=[C:27]([NH2:30])[N:26]=[CH:25][N:24]=3)=[C:19]([C:31]2[CH:36]=[CH:35][CH:34]=[CH:33][CH:32]=2)[N:18]=[CH:17]1.[CH:37]1(O)[CH2:42][CH2:41][CH2:40][CH2:39][CH2:38]1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1>C1COCC1>[CH:37]1([N:22]2[C:21]([C:20]3[N:16]([CH3:15])[CH:17]=[N:18][C:19]=3[C:31]3[CH:32]=[CH:33][CH:34]=[CH:35][CH:36]=3)=[N:29][C:28]3[C:23]2=[N:24][CH:25]=[N:26][C:27]=3[NH2:30])[CH2:42][CH2:41][CH2:40][CH2:39][CH2:38]1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 7966CyclohexanolHCID 11776TriphenylphosphineHCID 75555Diisopropyl diazene-1,2-dicarboxylateHCID 178481246HCID 178481246、化合物

生成物 1

HCID 103619899-Cyclohexyl-8-(1-methyl-4-phenyl-1H-imidazol-5-yl)-9H-purin-6-amine収率 11%

試薬・触媒・溶媒 1

HCID 8028
Tetrahydrofuran
溶媒

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%);

後処理

  1. temperaturewas heated at 40° C. for 48 hours
  2. waitat 55° C. for 24 hours
  3. customThe solvent was then evaporated in vacuo
  4. customto give a brown oil
  5. customPurification by preparative LCMS

出典と根拠

ORDレコード
ord-d48c83fc7ad5411db027175bd48b26b8
出典データセット
uspto-grants-2008_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07427616B2

反応ノート

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