HCID 23003686、化合物 → 3-Ethyl-4-hydroxy-3-methylpiperidine

HRID 396313ノート

反応式

HRID 396313 の反応式
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]

参加物

5

反応物 1

HCID 23003686HCID 23003686、化合物

生成物 1

HCID 230037053-Ethyl-4-hydroxy-3-methylpiperidine

試薬・触媒・溶媒 3

HCID 9942167Palladium hydroxide触媒HCID 887Methanol溶媒HCID 178418361HCID 178418361、化合物溶媒

実験手順

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).

後処理

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

出典と根拠

ORDレコード
ord-87c86658eece415095692f2d42104be7
出典データセット
uspto-grants-2003_08
特許番号
US06608078B2

反応ノート

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