Ethyl 3-methyl-4-(methylamino)-1-piperidinecarboxylate → N,3-Dimethylpiperidin-4-amine

HRID 1814854ノート

反応式

HRID 1814854 の反応式
C([N:6]1[CH2:11][CH2:10][CH:9]([NH:12][CH3:13])[CH:8]([CH3:14])[CH2:7]1)(OCC)=O>[OH-].[Na+]>[CH3:13][NH:12][CH:9]1[CH2:10][CH2:11][NH:6][CH2:7][CH:8]1[CH3:14]

参加物

3

反応物 1

HCID 15725099Ethyl 3-methyl-4-(methylamino)-1-piperidinecarboxylate

生成物 1

HCID 22278841N,3-Dimethylpiperidin-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-methylamino-3-methylpiperidine (4.0 g, 18.34 mmol) was suspended in 5 M NaOH solution (15 ml), stirred at 110° C. for 24 hr, cooled, extracted with ethyl acetate, dried (Na2SO4) and concentrated to dryness to afford 4-methylamino-3-methyl-piperidine. Yield 1.8 g (77%), C7H16N2, m/z 129 (M+1), PMR (CDCl3): 0.92 (dd, 3H), 1.54 (m, 1H), 2.12 (m, 2H), 2.38 (s, 3H), 2.6 (m, 1H), 2.8 (m, 1H), 3.02 (m,1H), 3.42 (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-42635a7587ba4679b1e96661f3637a2d
出典データセット
uspto-grants-2005_04
特許番号
US06878713B2

反応ノート

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