Methanol → HCID 24949336, 화합물

HRID 20876노트

반응식

HRID 20876 반응식
C(OC([N:8]1[CH2:12][CH2:11][CH2:10][C@H:9]1[C:13]1[NH:14][C:15]([C:18]2[CH:19]=[N:20][C:21]([C:24]3[CH:29]=[CH:28][C:27]([C:30]4[NH:31][C:32]([C@@H:35]5[CH2:39][CH2:38][CH2:37][N:36]5[C:40](=[O:53])[C@H:41]([NH:48][C:49]([O:51][CH3:52])=[O:50])[C:42]5[CH:47]=[CH:46][CH:45]=[CH:44][CH:43]=5)=[N:33][CH:34]=4)=[CH:26][CH:25]=3)=[N:22][CH:23]=2)=[CH:16][N:17]=1)=O)(C)(C)C.CO>CCOCC>[CH3:52][O:51][C:49](=[O:50])[NH:48][C@H:41]([C:42]1[CH:43]=[CH:44][CH:45]=[CH:46][CH:47]=1)[C:40](=[O:53])[N:36]1[CH2:37][CH2:38][CH2:39][C@H:35]1[C:32]1[NH:31][C:30]([C:27]2[CH:28]=[CH:29][C:24]([C:21]3[N:22]=[CH:23][C:18]([C:15]4[NH:14][C:13]([C@@H:9]5[CH2:10][CH2:11][CH2:12][NH:8]5)=[N:17][CH:16]=4)=[CH:19][N:20]=3)=[CH:25][CH:26]=2)=[CH:34][N:33]=1

참가 물질

4

반응물 2

HCID 887MethanolHCID 24951126(S)-2-{5-[2-(4-{2-[(S)-1-((R)-2-methoxycarbonylamino-2-phenyl-acetyl)-pyrrolidin-2-yl]-3H-imidazol-4-yl}-phenyl)-pyrimidin-5-yl]-1H-imidazol-2-yl}-pyrrolidine-1-carboxylic acid tert-butyl ester

생성물 1

HCID 24949336HCID 24949336, 화합물

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

실험 절차

Cold (0° C.) 4 NHCl in dioxanes (4 mL) was added via syringe to (S)-2-{5-[2-(4-{2-[(S)-1-((R)-2-methoxycarbonylamino-2-phenyl-acetyl)-pyrrolidin-2-yl]-3H-imidazol-4-yl}-phenyl)-pyrimidin-5-yl]-1H-imidazol-2-yl}-pyrrolidine-1-carboxylic acid tert-butyl ester (104.6 mg, 0.146 mmol) in a 100 mL pear-shaped flask followed by MeOH (0.5 mL). The homogeneous mixture was stirred at room temperature for 15 min before a precipitate was observed. After stirring further for 1.75 h, the suspension was diluted with ether and hexanes. Suction-filtration of a small portion of the suspension yielded the title compound as a yellow solid which was used for characterization purposes. The balance of the suspension was concentrated down to dryness and placed under high vacuum for 16 h. There was isolated the rest of the title compound also as a yellow solid (137.7 mg, 123%) which was used without further purification.

후처리

  1. stirringAfter stirring further for 1.75 h
  2. filtrationSuction-filtration of a small portion of the suspension

출처 및 근거

ORD 기록
ord-5ffee38320a447b98079c4d346eb95c2
출처 데이터셋
uspto-grants-2010_06
특허 번호
US07745636B2

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