Potassium Carbonate → Ethyl 1-(3-ethoxycarbonylpropylamino)cyclohexanecarboxylate

HRID 975838

反応式

HRID 975838 の反応式
[NH2:1][C:2]1([C:8]([O:10][CH2:11][CH3:12])=[O:9])[CH2:7][CH2:6][CH2:5][CH2:4][CH2:3]1.C(=O)([O-])[O-].[K+].[K+].Br[CH2:20][CH2:21][CH2:22][C:23]([O:25][CH2:26][CH3:27])=[O:24]>>[CH2:26]([O:25][C:23]([CH2:22][CH2:21][CH2:20][NH:1][C:2]1([C:8]([O:10][CH2:11][CH3:12])=[O:9])[CH2:7][CH2:6][CH2:5][CH2:4][CH2:3]1)=[O:24])[CH3:27]

参加物

4

反応物 3

HCID 11430Potassium CarbonateHCID 76300Ethyl 4-bromobutyrateHCID 222863Ethyl 1-aminocyclohexanecarboxylate

生成物 1

HCID 13282875Ethyl 1-(3-ethoxycarbonylpropylamino)cyclohexanecarboxylate

反応条件

温度
130 °C

実験手順

A mixture of ethyl 1-aminocyclohexanecarboxylate (669 g), potassium carbonate (683.1 g) and ethyl 4-bromobutyrate (558 ml) was stirred at 130° C. for 18 hours, then cooled to ambient temperature and poured onto ice-water (3 l). The product was extracted into dichloromethane and the combined extracts were dried over sodium sulphate and the solvent was removed in vacuo to yield ethyl 1-(3-ethoxycarbonylpropylamino)cyclohexanecarboxylate as a brown/orange oil. Yield 943.2 g.

後処理

  1. temperaturecooled to ambient temperature
  2. additionpoured onto ice-water (3 l)
  3. extractionThe product was extracted into dichloromethane
  4. dry with materialthe combined extracts were dried over sodium sulphate
  5. customthe solvent was removed in vacuo

出典と根拠

ORDレコード
ord-40fb88ba0f324bcc8f0a527c3d225990
出典データセット
uspto-grants-1997_03
特許番号
US05610161

関連ノート

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