1-Carbethoxy-4-dimethylamino-3-methylpiperidine → N,N,3-trimethylpiperidin-4-amine

HRID 1865229ノート

反応式

HRID 1865229 の反応式
C([N:6]1[CH2:11][CH2:10][CH:9]([N:12]([CH3:14])[CH3:13])[CH:8]([CH3:15])[CH2:7]1)(OCC)=O>[OH-].[Na+]>[CH3:13][N:12]([CH3:14])[CH:9]1[CH2:10][CH2:11][NH:6][CH2:7][CH:8]1[CH3:15]

参加物

3

反応物 1

HCID 222788651-Carbethoxy-4-dimethylamino-3-methylpiperidine

生成物 1

HCID 21973743N,N,3-trimethylpiperidin-4-amine

試薬・触媒・溶媒 1

HCID 14798Sodium Hydroxide溶媒

反応条件

温度
110 °C

実験手順

1-Carbethoxy-4-dimethylamino-3-methylpiperidine (3.5 g, 16.3 mmol) was suspended in 5 M NaOH solution (20 ml), stirred at 110° C. for 48 hr, cooled, extracted with ethyl acetate, dried (Na2SO4) and concentrated to dryness to afford 4-dimethylamino-3-methylpiperidine. Yield 1.0 g (43%), C8H18N2, m/z 143 (M+1), PMR (CDCl3): 0.96 (dd, 3H), 1.3 (m, 1H), 1.5 (m, 1H), 1.74 (m, 1H), 2.08 (m, 1H), 2.24 (s, 6H), 2.38 (m, 1H), 2.61 (bs, 1H, D2O exchangeable), 2.86 (m, 1H), 3.16 (m, 1H), 3.68 (m, 1H).

後処理

  1. temperaturecooled
  2. extractionextracted with ethyl acetate
  3. dry with materialdried (Na2SO4)
  4. concentrationconcentrated to dryness

出典と根拠

ORDレコード
ord-04df2f07ee314613a6ea6b4ed362a47c
出典データセット
uspto-grants-2009_12
特許番号
US07626032B2

反応ノート

読み込み中…