Potassium Carbonate → HCID 21202762、化合物

HRID 2223098ノート

反応式

HRID 2223098 の反応式
[NH:1]1[CH2:11][CH2:10][CH:4]([C:5]([O:7][CH2:8][CH3:9])=[O:6])[CH2:3][CH2:2]1.C(=O)([O-])[O-].[K+].[K+].[CH3:18][O:19][CH2:20][CH2:21]Br>C(O)C>[CH2:8]([O:7][C:5]([CH:4]1[CH2:3][CH2:2][N:1]([CH2:21][CH2:20][O:19][CH3:18])[CH2:11][CH2:10]1)=[O:6])[CH3:9]

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 70770Ethyl 4-piperidinecarboxylateHCID 809722-Bromoethyl methyl ether

生成物 1

HCID 21202762HCID 21202762、化合物収率 92%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A solution of ethyl isonipecotate (26 g, 166 mmol) in ethanol (150 ml) was treated with potassium carbonate (41 g, 297 mmol) and 2-bromoethyl methyl ether (25 g, 179 mmol). After heating at reflux for 24 hours, the mixture was filtered and the solid washed with ethanol. The filtrate was concentrated in vacuo to yield the title compound (32.76 g, 92%); 1H NMR (CDCl3) 4.12 (2H, q, J=7.1 Hz), 3.51 (2H, t, J=5.7 Hz), 3.33 (3H, s), 2.92 (2H, m), 2.56 (2H, t, J=5.7 Hz), 2.33-1.71 (7H, m) and 1.25 (3H, t, J7.1 Hz).

後処理

  1. temperatureAfter heating
  2. temperatureat reflux for 24 hours
  3. filtrationthe mixture was filtered
  4. washthe solid washed with ethanol
  5. concentrationThe filtrate was concentrated in vacuo

出典と根拠

ORDレコード
ord-faa11dca286a42819d4b0eff4f560e88
出典データセット
uspto-grants-2008_05
特許番号
US07375105B2

反応ノート

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