HCID 67059991、化合物 → 4-(2-Chlorophenyl)piperidine hydrochloride
反応式
[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[CH:8]1[CH2:13][CH2:12][N:11](C(=O)C)[CH2:10][CH2:9]1>[OH-].[Na+].C(O)C>[ClH:1].[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[CH:8]1[CH2:9][CH2:10][NH:11][CH2:12][CH2:13]1参加物
4
反応条件
- 温度
- 50 °C
実験手順
1-[4-(2-Chloro-phenyl)-piperidin-1-yl]-ethanone (0.2 g) was dissolved in a solution of aqueous sodium hydroxide (1 N, 5 mL) and ethanol (10 mL) and heated to 50° C. for 6 hours. The solvent was removed by evaporation under vacuum, and the products extracted into ethyl acetate, washed with water (20 mL) then dried over magnesium sulphate, filtered and the solvent removed by evaporation under vacuum. The residue was dissolved in a solution of hydrogen chloride in dioxane (4 N, 1 mL) and the solvent evaported to give the title compound as a pale yellow solid (0.12 g). LCMS m/z 196.1 [M+H]+. R.T.=2.46 min (Analytical Method 4).
後処理
- customThe solvent was removed by evaporation under vacuum
- extractionthe products extracted into ethyl acetate
- washwashed with water (20 mL)
- dry with materialthen dried over magnesium sulphate
- filtrationfiltered
- customthe solvent removed by evaporation under vacuum
- dissolutionThe residue was dissolved in a solution of hydrogen chloride in dioxane (4 N, 1 mL)
出典と根拠
- ORDレコード
- ord-584ad0baa6964a0190a1c5a728750e8c
- 出典データセット
- uspto-grants-2014_02
- 特許番号
- US08642621B2
反応ノート
読み込み中…