Hydrochloric Acid → 2-[(Methylsulfonyl)methyl]piperidine
反応式
[CH3:1][S:2]([CH2:5][C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][N:7]=1)(=[O:4])=[O:3].Cl>C(O)C.O=[Pt]=O>[CH3:1][S:2]([CH2:5][CH:6]1[CH2:11][CH2:10][CH2:9][CH2:8][NH:7]1)(=[O:4])=[O:3]参加物
5
実験手順
2-(Methylsulfonylmethyl)pyridine (4.40 g, 0.0257 moles) and PtO2 (0.50 g) were suspended in ethanol (80 mL) with 1N HCl (15 mL). The mixture was hydrogenated at 50 psi for 18 hours. The catalyst was filtered and the solvent removed. The residue was dissolved in CH2Cl2 and washed with sat. Na2CO3. The aqueous layer was extracted with CH2Cl2 (3×25 mL). The organic layers were combined and dried over Na2SO4 and evaporated to give a yellow oil (4.11 g, 90%) which solidified on standing. Further purification was unnecessary. LCMS (178, M+H).
後処理
- filtrationThe catalyst was filtered
- customthe solvent removed
- dissolutionThe residue was dissolved in CH2Cl2
- washwashed with sat. Na2CO3
- extractionThe aqueous layer was extracted with CH2Cl2 (3×25 mL)
- dry with materialdried over Na2SO4
- customevaporated
出典と根拠
- ORDレコード
- ord-13eb0f30e9ec42dd90368c66d1a9a5ac
- 出典データセット
- uspto-grants-2005_11
- 特許番号
- US06967196B1
反応ノート
読み込み中…