Methanol → 3-methoxy-2,2-dimethylpropionic acid 5-[[3-(2-acetoxyethoxy)-2-fluoro-5-methoxyphenyl]-(4-carbamimidoylphen ylamino)methyl]-2-pyrimidin-2-yl-2H-[1,2,4]triazol-3-yloxymethyl ester acetate

HRID 2089638

反応式

HRID 2089638 の反応式
[C:1]([O:4][CH2:5][CH2:6][O:7][C:8]1[C:9]([F:57])=[C:10]([CH:16]([NH:39][C:40]2[CH:45]=[CH:44][C:43]([C:46]([NH2:56])=[N:47]C(=O)C3C=CC=CC=3)=[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].CO>C(O)(=O)C>[C:1]([OH:4])(=[O:3])[CH3:2].[C:1]([O:4][CH2:5][CH2:6][O:7][C:8]1[C:9]([F:57])=[C:10]([CH:16]([NH:39][C:40]2[CH:45]=[CH:44][C:43]([C:46](=[NH:47])[NH2:56])=[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]

参加物

4

反応物 2

HCID 887MethanolHCID 674705203-methoxy-2,2-dimethylpropionic acid 5-[[3-(2-acetoxyethoxy)-2-fluoro-5-methoxyphenyl]-(4-{amino[benzoylimino]methyl}phenylamino)methyl]-2-pyrimidin-2-yl-2H-[1,2,4]triazol-3-yloxymethyl ester

生成物 1

HCID 674699453-methoxy-2,2-dimethylpropionic acid 5-[[3-(2-acetoxyethoxy)-2-fluoro-5-methoxyphenyl]-(4-carbamimidoylphen ylamino)methyl]-2-pyrimidin-2-yl-2H-[1,2,4]triazol-3-yloxymethyl ester acetate収率 168.1%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

反応条件

温度
40 °C

実験手順

Under nitrogen atmosphere, a mixture of 3-methoxy-2,2-dimethylpropionic acid 5-[[3-(2-acetoxyethoxy)-2-fluoro-5-methoxyphenyl]-(4-{amino[benzoylimino]methyl}phenylamino)methyl]-2-pyrimidin-2-yl-2H-[1,2,4]triazol-3-yloxymethyl ester (184 mg), methanol (10 mL), and acetic acid (1 mL) was stirred at 40° C. for 15 hours. Under reduced pressure, the solvent in the mixture was distilled off. The residue obtained was purified by reverse phase silica gel column chromatography (mixed solvent of acetonitrile-water, containing 0.1% of acetic acid) to obtain the captioned compound (146 mg).

後処理

  1. distillationUnder reduced pressure, the solvent in the mixture was distilled off
  2. customThe residue obtained
  3. customwas purified by reverse phase silica gel column chromatography (mixed solvent of acetonitrile-water, containing 0.1% of acetic acid)

出典と根拠

ORDレコード
ord-09cbbe893859437d9856ece28bb70eb6
出典データセット
uspto-grants-2013_05
特許番号
US08436009B2

関連ノート

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