1,1'-Carbonyldiimidazole → HCID 66634907、化合物

HRID 510113ノート

反応式

HRID 510113 の反応式
[NH2:1][C:2]1[C:7]([OH:8])=[C:6]([NH2:9])[N:5]=[C:4]([C:10]2[C:18]3[C:13](=[N:14][CH:15]=[CH:16][CH:17]=3)[N:12]([CH2:19][C:20]3[CH:25]=[CH:24][CH:23]=[CH:22][C:21]=3[F:26])[N:11]=2)[N:3]=1.C(N(CC)C(C)C)(C)C.[C:36](N1C=CN=C1)(N1C=CN=C1)=[O:37]>CN(C)C=O>[NH2:9][C:6]1[C:7]2[O:8][C:36](=[O:37])[NH:1][C:2]=2[N:3]=[C:4]([C:10]2[C:18]3[C:13](=[N:14][CH:15]=[CH:16][CH:17]=3)[N:12]([CH2:19][C:20]3[CH:25]=[CH:24][CH:23]=[CH:22][C:21]=3[F:26])[N:11]=2)[N:5]=1

参加物

5

反応物 3

HCID 682631,1'-CarbonyldiimidazoleHCID 81531DiisopropylethylamineHCID 136364529HCID 136364529、化合物

生成物 1

HCID 66634907HCID 66634907、化合物収率 52.7%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

159 mg (0.453 mmol) of the compound prepared in example 58A in dimethylformamide (10 ml) were admixed with 94 μl (0.543 mmol) of N,N-diisopropylethylamine and 88 mg (0.543 mmol) of carbonyldiimidazole, and the mixture was stirred at RT overnight. The mixture was filtered, the filtrate was concentrated and the residue was purified by means of preparative HPLC (acetonitrile:water (+0.05% formic acid) gradient). 90 mg of the title compound were obtained (52% of theory).

後処理

  1. filtrationThe mixture was filtered
  2. concentrationthe filtrate was concentrated
  3. customthe residue was purified by means of preparative HPLC (acetonitrile:water (+0.05% formic acid) gradient)

出典と根拠

ORDレコード
ord-0ed241d160c34e2c870057e5f5c41d72
出典データセット
uspto-grants-2015_08
特許番号
US09096592B2

反応ノート

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