2,2-Diphenylethylamine → (1-{(1S,4R)-4-[2-Chloro-6-(2,2-diphenylethylamino)-purin-9-yl]-cyclopent-2-enyl}-1H-pyrazol-4-yl)-methanol

HRID 655132ノート

反応式

HRID 655132 の反応式
[Cl:1][C:2]1[N:10]=[C:9]2[C:5]([N:6]=[CH:7][N:8]2[C@@H:11]2[CH2:15][C@H:14]([N:16]3[CH:20]=[C:19]([CH2:21][OH:22])[CH:18]=[N:17]3)[CH:13]=[CH:12]2)=[C:4](Cl)[N:3]=1.[C:24]1([CH:30]([C:33]2[CH:38]=[CH:37][CH:36]=[CH:35][CH:34]=2)[CH2:31][NH2:32])[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1.CCN(C(C)C)C(C)C>C1COCC1>[Cl:1][C:2]1[N:10]=[C:9]2[C:5]([N:6]=[CH:7][N:8]2[C@@H:11]2[CH2:15][C@H:14]([N:16]3[CH:20]=[C:19]([CH2:21][OH:22])[CH:18]=[N:17]3)[CH:13]=[CH:12]2)=[C:4]([NH:32][CH2:31][CH:30]([C:24]2[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=2)[C:33]2[CH:38]=[CH:37][CH:36]=[CH:35][CH:34]=2)[N:3]=1

参加物

5

反応物 3

HCID 775752,2-DiphenylethylamineHCID 81531DiisopropylethylamineHCID 86637576{1-[(1S,4R)-4-(2,6-Dichloro-purin-9-yl)cyclopent-2-enyl]-1H-pyrazol-4-yl}-methanol

生成物 1

HCID 86645704(1-{(1S,4R)-4-[2-Chloro-6-(2,2-diphenylethylamino)-purin-9-yl]-cyclopent-2-enyl}-1H-pyrazol-4-yl)-methanol

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

A mixture comprising {1-[(1S,4R)-4-(2,6-dichloro purin-9-yl)-cyclopent-2-enyl]-1H-pyrazol-4-yl}-methanol (0.675 g, 1.92 mmol), diphenylethylamine (0.398 g, 2.02 mmol) and DIPEA (0.298 g, 2.31 mmol) in dry THF (20 mL) is stirred at 35 C for 3 days. The solvent is removed in vacuo and the resulting crude residue is partitioned between DCM and 0.1 M HCl. The organic portion is separated, washed with water, brine, dried (MgSO4) and concentrated in vacuo to afford the title product.

後処理

  1. customThe solvent is removed in vacuo
  2. customthe resulting crude residue is partitioned between DCM and 0.1 M HCl
  3. customThe organic portion is separated
  4. washwashed with water, brine
  5. dry with materialdried (MgSO4)
  6. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-0905fb1ade4b4b02a95975cfbb8e738e
出典データセット
uspto-grants-2011_12
特許番号
US08071565B2

反応ノート

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