Acetamidomalonic acid diethyl ester → Diethyl 2-acetamido-2-(9-octadecenyl)malonate

HRID 617831

反応式

HRID 617831 の反応式
[C:1]([NH:4][CH:5]([C:11]([O:13][CH2:14][CH3:15])=[O:12])[C:6]([O:8][CH2:9][CH3:10])=[O:7])(=[O:3])[CH3:2].[O-]CC.[Na+].[CH2:20](Cl)[CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH:28]=[CH:29][CH2:30][CH2:31][CH2:32][CH2:33][CH2:34][CH2:35][CH2:36][CH3:37]>C(O)C>[C:1]([NH:4][C:5]([CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH:28]=[CH:29][CH2:30][CH2:31][CH2:32][CH2:33][CH2:34][CH2:35][CH2:36][CH3:37])([C:11]([O:13][CH2:14][CH3:15])=[O:12])[C:6]([O:8][CH2:9][CH3:10])=[O:7])(=[O:3])[CH3:2]

参加物

5

反応物 3

HCID 14041Acetamidomalonic acid diethyl esterHCID 5580461-Chlorooctadec-9-eneHCID 2723922Sodium ethoxide

生成物 1

HCID 53823167Diethyl 2-acetamido-2-(9-octadecenyl)malonate収率 4%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒2 回

実験手順

Diethyl 2-acetamidomalonate (15 g) was dissolved in 200 ml of dry ethanol and 5.6 g of sodium ethoxide was added thereto. To the reaction mixture, 22 g of 9-octadecenyl chloride was added while stirring at room temperature. The inside of the reaction vessel was displaced with nitrogen and the mixture was refluxed for about 15 hours. The mixture was neutralized with ethanol-concentrated hydrochloric acid (11:1) and concentrated. The concentrate was purified by silica gel column chromatography to give 1.3 g of diethyl 2-acetamido-2-(9-octadecenyl)malonate as a colorless, oily and viscous substance.

後処理

  1. temperaturethe mixture was refluxed for about 15 hours
  2. concentrationconcentrated
  3. customThe concentrate was purified by silica gel column chromatography

出典と根拠

ORDレコード
ord-71774a56c2204d35985395e3ab488a1a
出典データセット
uspto-grants-1999_09
特許番号
US05952316

関連ノート

読み込み中…