反応式
[OH-].[Li+].[Cl:3][C:4]1[N:5]=[C:6]([C:11]([NH:13][C@H:14]2[CH2:19][CH2:18][N:17]([C:20]3[S:21][C:22]([C:26]([O:28]CC)=[O:27])=[C:23]([CH3:25])[N:24]=3)[CH2:16][C@H:15]2[F:31])=[O:12])[NH:7][C:8]=1[CH2:9][CH3:10].Cl.O>CO.O1CCCC1>[Cl:3][C:4]1[N:5]=[C:6]([C:11]([NH:13][C@H:14]2[CH2:19][CH2:18][N:17]([C:20]3[S:21][C:22]([C:26]([OH:28])=[O:27])=[C:23]([CH3:25])[N:24]=3)[CH2:16][C@H:15]2[F:31])=[O:12])[NH:7][C:8]=1[CH2:9][CH3:10]参加物
反応物 4
生成物 1
試薬・触媒・溶媒 2
反応条件
- 温度
- 70 °C
実験手順
A 2 N aqueous lithium hydroxide solution (1.18 mL, 2.37 mmol) was added to a mixed solution of ethyl cis(±)-2-(4-{[(4-chloro-5-ethyl-1H-imidazol-2-yl)carbonyl]amino}-3-fluoropiperidin-1-yl)-4-methyl-1,3-thiazole-5-carboxylate obtained in Example (196c) (105 mg, 0.237 mmol) in methanol (3 mL) and tetrahydrofuran (3 mL) at room temperature, and the mixture was stirred at 70° C. for two hours. The reaction solution was concentrated under reduced pressure. A 1 N aqueous hydrochloric acid solution (2.37 mL, 2.37 mmol) and water were added to the resulting residue, followed by extraction with ethyl acetate. The resulting organic layer was washed with water and brine, and dried over anhydrous sodium sulfate, and then the insoluble matter was separated by filtration. The filtrate was concentrated under reduced pressure to obtain 72 mg of the title compound (73%) as a colorless solid.
後処理
- concentrationThe reaction solution was concentrated under reduced pressure
- extractionfollowed by extraction with ethyl acetate
- washThe resulting organic layer was washed with water and brine
- dry with materialdried over anhydrous sodium sulfate
- customthe insoluble matter was separated by filtration
- concentrationThe filtrate was concentrated under reduced pressure
出典と根拠
- ORDレコード
- ord-ddc5bd76f1e84cf5a54a4d4f1ca44748
- 出典データセット
- uspto-grants-2015_01
- 特許番号
- US08927588B2
関連ノート
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