反応式
C(OC([N:8]1[CH:13]2[CH2:14][CH2:15][CH:9]1[CH2:10][CH:11]([C:16]1[CH:21]=[CH:20][C:19]([N:22]3[CH2:27][CH2:26][N:25]([S:28]([CH3:31])(=[O:30])=[O:29])[CH2:24][CH2:23]3)=[CH:18][CH:17]=1)[CH2:12]2)=O)(C)(C)C.Cl.O1CCOCC1>ClCCl>[CH3:31][S:28]([N:25]1[CH2:24][CH2:23][N:22]([C:19]2[CH:18]=[CH:17][C:16]([CH:11]3[CH2:10][CH:9]4[NH:8][CH:13]([CH2:14][CH2:15]4)[CH2:12]3)=[CH:21][CH:20]=2)[CH2:27][CH2:26]1)(=[O:29])=[O:30]参加物
反応物 3
生成物 1
試薬・触媒・溶媒 1
実験手順
3-[4-(4-Methanesulfonylpiperazin-1-yl)phenyl]-8-azabicyclo[3.2.1]octane-8-carboxylic acid tert-butyl ester (0.758 g, 1.69 mmol) is solubilized in 158 ml of dichloromethane. 4N HCl in dioxane (4.2 ml, 16.8 mmol) is then added. After stirring for 16 h at ambient temperature, the reaction medium is concentrated, taken up with water, and washed with ethyl acetate. The pH of the aqueous phase is then adjusted to 10 with a 5N aqueous solution of sodium hydroxide. After extraction with dichloromethane, and washing with water and then with a saturated aqueous sodium chloride solution, the organic phase is dried over MgSO4 and then concentrated to dryness. 0.51 g of expected 3-[4-(4-methanesulfonylpiperazin-1-yl)phenyl]-8-aza-bicyclo[3.2.1]octane is obtained, which is subsequently used as it is.
後処理
- concentrationthe reaction medium is concentrated
- washwashed with ethyl acetate
- extractionAfter extraction with dichloromethane
- washwashing with water
- dry with materialwith a saturated aqueous sodium chloride solution, the organic phase is dried over MgSO4
- concentrationconcentrated to dryness
出典と根拠
- ORDレコード
- ord-479e70835b7d462194d5dd9b232e2334
- 出典データセット
- uspto-grants-2013_09
- 特許番号
- US08530477B2
関連ノート
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