Methanol → HCID 24949336、化合物

HRID 80373ノート

反応式

HRID 80373 の反応式
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

参加物

4

反応物 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

生成物 1

HCID 24949336HCID 24949336、化合物

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-217b67edb69743478d9f21c4db2fae63
出典データセット
uspto-grants-2014_09
特許番号
US08846023B2

反応ノート

読み込み中…