Hydrochloric Acid → 1-(2-Methoxyethyl)piperidine-4-carboxylic acid hydrochloride
반응식
[ClH:1].C([O:4][C:5]([CH:7]1[CH2:12][CH2:11][N:10]([CH2:13][CH2:14][O:15][CH3:16])[CH2:9][CH2:8]1)=[O:6])C>O>[ClH:1].[CH3:16][O:15][CH2:14][CH2:13][N:10]1[CH2:9][CH2:8][CH:7]([C:5]([OH:6])=[O:4])[CH2:12][CH2:11]1참가 물질
4
반응 조건
- 온도
- 100 °C
실험 절차
Concentrated hydrochloric acid (200 ml) was added to a suspension of the product of Example 4 Step 1 (20 g, 93 mmol) in water (120 ml). The mixture was heated at 100° C. for 60 hours, cooled to room temperature and the solvent concentrated in vacuo. The residue was azeotroped with toluene (×5) and dried over phosphorus pentoxide. The resulting solid was triturated with diethyl ether and acetone to yield the title compound (14.0 g, 81%); MS (ES−) m/e 186 [M−H]−.
후처리
- temperaturecooled to room temperature
- concentrationthe solvent concentrated in vacuo
- customThe residue was azeotroped with toluene (×5)
- dry with materialdried over phosphorus pentoxide
- customThe resulting solid was triturated with diethyl ether and acetone
출처 및 근거
- ORD 기록
- ord-149512a843244560b5576b09c2d5fb78
- 출처 데이터셋
- uspto-grants-2008_05
- 특허 번호
- US07375105B2
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