Hydrochloric Acid → Methyl cis(+/-)-2-acetyl-4-(4-{[(benzyloxy)carbonyl]amino}-3-methoxypiperidin-1-yl)-4-oxobutanoate
反応式
[C:1]([O:7][CH3:8])(=[O:6])[CH2:2][C:3]([CH3:5])=[O:4].C[O-].[Na+].Cl[CH2:13][C:14]([N:16]1[CH2:21][CH2:20][C@H:19]([NH:22][C:23](=[O:32])[O:24][CH2:25][C:26]2[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=2)[C@H:18]([O:33][CH3:34])[CH2:17]1)=[O:15].Cl>CO.C(OCC)(=O)C>[C:3]([CH:2]([CH2:13][C:14]([N:16]1[CH2:21][CH2:20][C@H:19]([NH:22][C:23]([O:24][CH2:25][C:26]2[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=2)=[O:32])[C@H:18]([O:33][CH3:34])[CH2:17]1)=[O:15])[C:1]([O:7][CH3:8])=[O:6])(=[O:4])[CH3:5]参加物
7
反応物 4
生成物 1
試薬・触媒・溶媒 2
実験手順
Methyl acetoacetate (510 mg, 4.4 mmol) was dissolved in methanol (15 ml). Sodium methoxide (210 mg, 3.9 mmol) was added, and the mixture was stirred at room temperature for 30 minutes. Further, benzyl cis(±)-[1-(chloroacetyl)-3-methoxypiperidin-4-yl]carbamate obtained in Example (188a) was dissolved in methanol (10 ml). The solution was added to the reaction solution, and the mixture was stirred at 70° C. overnight. The reaction solution was diluted with ethyl acetate, neutralized with 1 N hydrochloric acid, washed with brine, and dried over anhydrous sodium sulfate. Following concentration under reduced pressure, the title compound was obtained. The resulting compound was used for the next reaction without purification.
後処理
- additionThe solution was added to the reaction solution
- stirringthe mixture was stirred at 70° C. overnight
- washwashed with brine
- dry with materialdried over anhydrous sodium sulfate
- concentrationconcentration under reduced pressure
出典と根拠
- ORDレコード
- ord-995aeebb84ef474ca6da894eb038396b
- 出典データセット
- uspto-grants-2015_01
- 特許番号
- US08927588B2
反応ノート
読み込み中…