反応式
CO[C@H](C1C=CC=CC=1)C(O)=O.[F:13][C:14]1[C:19]([O:20][CH2:21][CH2:22][OH:23])=[CH:18][C:17]([O:24][CH3:25])=[CH:16][C:15]=1[C@@H:26]([NH:39][C:40]1[CH:48]=[CH:47][C:43]([C:44]([NH2:46])=[NH:45])=[CH:42][CH:41]=1)[C:27]1[NH:31][C:30](=[O:32])[N:29]([C:33]2[N:38]=[CH:37][CH:36]=[CH:35][N:34]=2)[N:28]=1.CO.[ClH:51]>C(O)C>[ClH:51].[F:13][C:14]1[C:19]([O:20][CH2:21][CH2:22][OH:23])=[CH:18][C:17]([O:24][CH3:25])=[CH:16][C:15]=1[C@@H:26]([NH:39][C:40]1[CH:41]=[CH:42][C:43]([C:44]([NH2:46])=[NH:45])=[CH:47][CH:48]=1)[C:27]1[NH:31][C:30](=[O:32])[N:29]([C:33]2[N:34]=[CH:35][CH:36]=[CH:37][N:38]=2)[N:28]=1参加物
5
反応物 3
生成物 1
試薬・触媒・溶媒 1
実験手順
To a mixture of 4-{[(R)-[2-fluoro-3-(2-hydroxyethoxy)-5-methoxyphenyl](5-oxo-1-pyrimidin-2-yl-4,5-dihydro-1H-1,2,4-triazol-3-yl)methyl]amino}benzamidine (R)-methoxyphenylacetate (20 g, 30.2 mmol), methanol (200 mL), and ethanol (400 mL), 5 N hydrochloric acid (20 mL, 100 mmol) was added to dissolve the same. A seed crystal of the captioned compound was added to the reaction solution, and the resulting mixture was stirred overnight at room temperature. The precipitated solid was filtered and sequentially washed with a mixed solvent of ethanol and methanol (ethanol:methanol=2:1, 50 mL) and tert-butyl methyl ether (50 mL). The solid obtained was dried under air flow to obtain the captioned compound (14.52 g) as a white solid.
後処理
- additionwas added
- dissolutionto dissolve the same
- additionA seed crystal of the captioned compound was added to the reaction solution
- filtrationThe precipitated solid was filtered
- washsequentially washed with a mixed solvent of ethanol and methanol (ethanol:methanol=2:1, 50 mL) and tert-butyl methyl ether (50 mL)
- customThe solid obtained
- customwas dried under air flow
出典と根拠
- ORDレコード
- ord-3f7cb31ff46c4440be0c778663882283
- 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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