Potassium Hydroxide → 3543-21-3

HRID 2387952ノート

反応式

HRID 2387952 の反応式
[OH-].[K+].C(OC([N:13]1[CH2:18][CH2:17][C:16]([C:24]2[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=2)([N:19]2[CH2:23][CH2:22][CH2:21][CH2:20]2)[CH2:15][CH2:14]1)=O)C1C=CC=CC=1.CO.C(Cl)(Cl)Cl>C(O)C>[C:24]1([C:16]2([N:19]3[CH2:20][CH2:21][CH2:22][CH2:23]3)[CH2:15][CH2:14][NH:13][CH2:18][CH2:17]2)[CH:25]=[CH:26][CH:27]=[CH:28][CH:29]=1

参加物

5

反応物 3

HCID 14797Potassium HydroxideHCID 21584188Chloroform methanolHCID 67366133HCID 67366133、化合物

生成物 1

HCID 594016893543-21-3収率 151.7%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

11 g of KOH were added to a solution of 7.3 g (1 equiv.) of benzyloxycarbonyl-4-phenyl-4-(pyrrolidin-1-yl)piperidine in 100 ml of ethanol, and the reaction mixture was heated for 24 hours at reflux. The progress of the reaction was monitored by thin-layer chromatography (20% MeOH/CHCl3). When the reaction was complete, the solvent was distilled off completely, 100 ml of water were added to the residue, and extraction was carried out 3× with 100 ml of CHCl3. The combined organic phases were dried with Na2SO4. After removal of the solvent under reduced pressure, 7 g of crude product were obtained in the form of an oil.

後処理

  1. temperaturethe reaction mixture was heated for 24 hours
  2. temperatureat reflux
  3. distillationthe solvent was distilled off completely
  4. addition100 ml of water were added to the residue, and extraction
  5. dry with materialThe combined organic phases were dried with Na2SO4
  6. customAfter removal of the solvent under reduced pressure

出典と根拠

ORDレコード
ord-baa4d7cc115d45bdbacd158e022d9ddf
出典データセット
uspto-grants-2012_09
特許番号
US08269000B2

反応ノート

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