1,1'-Carbonyldiimidazole → HCID 66634907, 화합물

HRID 510113노트

반응식

HRID 510113 반응식
[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

참가 물질

5

반응물 3

HCID 682631,1'-CarbonyldiimidazoleHCID 81531DiisopropylethylamineHCID 136364529HCID 136364529, 화합물

생성물 1

HCID 66634907HCID 66634907, 화합물수율 52.7%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

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).

후처리

  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)

출처 및 근거

ORD 기록
ord-0ed241d160c34e2c870057e5f5c41d72
출처 데이터셋
uspto-grants-2015_08
특허 번호
US09096592B2

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