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Diazald → HCID 53380262, 화합물

HRID 2388602
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HRID 2388602 반응식
[OH-].[K+].[CH3:3]C1C=CC(S(N(N=O)C)(=O)=O)=CC=1.C(O)CO.CCOCC.[NH:26]1[C:30]2[CH:31]=[C:32]([N:35]3[CH:39]([C:40]4[CH:45]=[CH:44][C:43]([C:46]5[CH:51]=[CH:50][CH:49]=[CH:48][CH:47]=5)=[CH:42][CH:41]=4)[C:38]([CH3:52])=[C:37]([OH:53])[C:36]3=[O:54])[CH:33]=[CH:34][C:29]=2[N:28]=[CH:27]1>CO>[NH:26]1[C:30]2[CH:31]=[C:32]([N:35]3[CH:39]([C:40]4[CH:41]=[CH:42][C:43]([C:46]5[CH:51]=[CH:50][CH:49]=[CH:48][CH:47]=5)=[CH:44][CH:45]=4)[C:38]([CH3:52])=[C:37]([O:53][CH3:3])[C:36]3=[O:54])[CH:33]=[CH:34][C:29]=2[N:28]=[CH:27]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 6628DiazaldHCID 14797Potassium HydroxideHCID 21225595HCID 21225595, 화합물HCID 131729952HCID 131729952, 화합물

생성물 1

HCID 53380262HCID 53380262, 화합물

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

The compound was synthesized starting from KOH (15 eq in water), diazald (8 eq), ethylene glycol/Et2O (1/2 v/v, 60 ml), 1-(1H-Benzo[d]imidazol-6-yl)-3-hydroxy-4-methyl-5-(biphen-4-yl)-1H-pyrrol-2(5H)-one (1 g, 2.63 mmol, 1 eq) and MeOH (20 ml); yield 0.070 g (17.7%); MS m/z: 396.1 [M+H]+; 1H-NMR: (400 MHz, DMSO-D6) δ: 12.39 (s, 1H), 8.14 (s, 1H), 7.76-7.72 (m, 1H), 7.59-7.28 (m, 11H), 5.88 (s, 1H), 3.96 (s, 3H),1.75 (s, 3H); HPLC (METHOD [A]): rt 14.00 min (98.38%)

후처리

  1. customThe compound was synthesized
  2. customrt 14.00 min (98.38%)

출처 및 근거

ORD 기록
ord-34e6c3bd1b0144e58bb9d5d66de3e4ba
출처 데이터셋
uspto-grants-2012_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08269019B2

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