HCID 70028630, 화합물 → HCID 45083227, 화합물

HRID 396321노트

반응식

HRID 396321 반응식
C([N:8]1[CH2:13][CH2:12][CH:11]([OH:14])[CH:10]([CH2:15][CH2:16][CH2:17][CH3:18])[CH2:9]1)C1C=CC=CC=1>CO.[H][H].[OH-].[Pd+2].[OH-]>[CH2:15]([CH:10]1[CH:11]([OH:14])[CH2:12][CH2:13][NH:8][CH2:9]1)[CH2:16][CH2:17][CH3:18]

참가 물질

5

반응물 1

HCID 70028630HCID 70028630, 화합물

생성물 1

HCID 45083227HCID 45083227, 화합물

시약·촉매·용매 3

HCID 9942167Palladium hydroxide촉매HCID 887Methanol용매HCID 178418361HCID 178418361, 화합물용매

실험 절차

A mixture of 1-benzyl-3-n-butyl-4-hydroxypiperidine (2.5 g, 10.0 mmole) and 20% palladium hydroxide (0.2 g) in methanol (25 ml) was stirred in hydrogen atmosphere (1 atm.) for 24 hr at 30° C. Catalyst was filtered off, washed with methanol, filtrate was concentrated to dryness to give 3-n-butyl-4-hydroxypiperidine as oil. Yield 1.4 g (87%), C9H19NO, m/z 158 (M+1) PMR (CDCl3): 0.94 (3H, t, CH3, j=8 Hz), 1.04-1.54 (7H, m, 3×CH2 & H3), 1.74 (1H, m, H5), 1.98 (2H, m, H5, & OH, D2O exchangeable), 2.22 (1H, m, H2), 2.7 (1H, m, H6), 3.12 (1H, m, H2), 3.3 (1H, m, H6), 3.46 (1H, bs, NH, D2O exchangeable), 3.98 (1H, m, H4).

후처리

  1. filtrationCatalyst was filtered off
  2. washwashed with methanol, filtrate
  3. concentrationwas concentrated to dryness

출처 및 근거

ORD 기록
ord-dd458bf80ad14a809bbb92813067d02e
출처 데이터셋
uspto-grants-2003_08
특허 번호
US06608078B2

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