HCID 23003686, 화합물 → 3-Ethyl-4-hydroxy-3-methylpiperidine
반응식
C([N:8]1[CH2:13][CH2:12][CH:11]([OH:14])[C:10]([CH2:16][CH3:17])([CH3:15])[CH2:9]1)C1C=CC=CC=1>CO.[H][H].[OH-].[Pd+2].[OH-]>[CH2:16]([C:10]1([CH3:15])[CH:11]([OH:14])[CH2:12][CH2:13][NH:8][CH2:9]1)[CH3:17]참가 물질
5
실험 절차
A mixture of 1-benzyl-3-ethyl-4-hydroxy-3-methylpiperidine (1.1 g, 4.74 mmole) and 20% palladium hydroxide (0.4 g) in methanol (20 ml) was stirred at ambient temperature in hydrogen atmosphere (1 atm.) for 20 hr. Catalyst was filtered off, washed with methanol, filtrate was concentrated to dryness to give 3-ethyl-4-hydroxy-3-methylpiperidine as oil. Yield 0.6 g (90%), C8H17NO, m/z 144 (M+1), PMR (CDCl3): 0.7-1.06 (6H, m, 2×CH3), 1.24-2.0 (5H, m, CH2, H5, NH & OH, NH & OH D2O exchangeable), 2.3 (1H, m, H5), 2.62-3.18 (2H, m, H2), 3.3-3.8 (3H, m, H4 & H6).
후처리
- filtrationCatalyst was filtered off
- washwashed with methanol, filtrate
- concentrationwas concentrated to dryness
출처 및 근거
- ORD 기록
- ord-87c86658eece415095692f2d42104be7
- 출처 데이터셋
- uspto-grants-2003_08
- 특허 번호
- US06608078B2
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