Toluene → 3-methoxy-2,2-dimethylpropionic acid 5-[(R)-[3-(2-acetoxyethoxy)-2-fluoro-5-methoxyphenyl]-(4-{amino[2-methylallyloxycarbonylimino]methyl}phenylamino)methyl]-2-pyrimidin-2-yl-2H-[1,2,4]triazol-3-yloxymethyl ester hydrochloride

HRID 2089672ノート

反応式

HRID 2089672 の反応式
[C:1]([O:4][CH2:5][CH2:6][O:7][C:8]1[C:9]([F:56])=[C:10]([C@@H:16]([NH:39][C:40]2[CH:45]=[CH:44][C:43]([C:46]([NH2:55])=[N:47][C:48]([O:50][CH2:51][C:52]([CH3:54])=[CH2:53])=[O:49])=[CH:42][CH:41]=2)[C:17]2[N:18]=[C:19]([O:28][CH2:29][O:30][C:31](=[O:38])[C:32]([CH3:37])([CH3:36])[CH2:33][O:34][CH3:35])[N:20]([C:22]3[N:27]=[CH:26][CH:25]=[CH:24][N:23]=3)[N:21]=2)[CH:11]=[C:12]([O:14][CH3:15])[CH:13]=1)(=[O:3])[CH3:2].C1(C)C=CC=CC=1.C(OCC)(=O)C.[ClH:70]>C(OCC)(=O)C>[ClH:70].[C:1]([O:4][CH2:5][CH2:6][O:7][C:8]1[C:9]([F:56])=[C:10]([C@@H:16]([NH:39][C:40]2[CH:41]=[CH:42][C:43]([C:46]([NH2:55])=[N:47][C:48]([O:50][CH2:51][C:52]([CH3:54])=[CH2:53])=[O:49])=[CH:44][CH:45]=2)[C:17]2[N:18]=[C:19]([O:28][CH2:29][O:30][C:31](=[O:38])[C:32]([CH3:37])([CH3:36])[CH2:33][O:34][CH3:35])[N:20]([C:22]3[N:27]=[CH:26][CH:25]=[CH:24][N:23]=3)[N:21]=2)[CH:11]=[C:12]([O:14][CH3:15])[CH:13]=1)(=[O:3])[CH3:2]

参加物

5

反応物 3

HCID 1140TolueneHCID 21866389Hydrogen chloride-ethyl acetateHCID 674711843-methoxy-2,2-dimethylpropionic acid 5-[(R)-[3-(2-acetoxyethoxy)-2-fluoro-5-methoxyphenyl]-(4-{amino[2-methylallyloxycarbonylimino]methyl}phenylamino)methyl]-2-pyrimidin-2-yl-2H-[1,2,4]triazol-3-yloxymethyl ester

生成物 1

HCID 866774043-methoxy-2,2-dimethylpropionic acid 5-[(R)-[3-(2-acetoxyethoxy)-2-fluoro-5-methoxyphenyl]-(4-{amino[2-methylallyloxycarbonylimino]methyl}phenylamino)methyl]-2-pyrimidin-2-yl-2H-[1,2,4]triazol-3-yloxymethyl ester hydrochloride

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

To a mixture of 3-methoxy-2,2-dimethylpropionic acid 5-[(R)-[3-(2-acetoxyethoxy)-2-fluoro-5-methoxyphenyl]-(4-{amino[2-methylallyloxycarbonylimino]methyl}phenylamino)methyl]-2-pyrimidin-2-yl-2H-[1,2,4]triazol-3-yloxymethyl ester (Example 6f, 20 mg) and toluene (4 mL), under stirring at room temperature, a dilution (0.2 mL) prepared by adding 4 M hydrogen chloride-ethyl acetate solution (0.32 mL) to ethyl acetate (10 mL) was added dropwise. The solvent in the mixture was distilled off under reduced pressure to obtain the captioned compound (20 mg).

後処理

  1. customa dilution (0.2 mL) prepared
  2. additionwas added dropwise
  3. distillationThe solvent in the mixture was distilled off under reduced pressure

出典と根拠

ORDレコード
ord-6e7e59512816409d9da19341f9b036aa
出典データセット
uspto-grants-2013_05
特許番号
US08436009B2

反応ノート

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