Methanol → Diethyl 2-acetamido-2-(2-pentadecynyl)malonate

HRID 862829ノート

反応式

HRID 862829 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].[CH3:16][CH2:17][O-].[Na+].[CH2:20]([C:28]1[CH:33]=[CH:32][C:31](CCO)=[CH:30][CH:29]=1)[CH2:21][CH2:22][CH2:23][CH2:24][CH2:25][CH2:26]C.CO>C(O)C>[C:1]([NH:4][C:5]([CH2:26][C:25]#[C:24][CH2:23][CH2:22][CH2:21][CH2:20][CH2:28][CH2:29][CH2:30][CH2:31][CH2:32][CH2:33][CH2:17][CH3:16])([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

6

反応物 4

HCID 887MethanolHCID 14041Acetamidomalonic acid diethyl esterHCID 2723922Sodium ethoxideHCID 113108762-(4-Octylphenyl)ethanol

生成物 1

HCID 21849278Diethyl 2-acetamido-2-(2-pentadecynyl)malonate

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒2 回

実験手順

Diethyl acetamidomalonate (3.327 g) and 1.137 g of sodium ethylate were dissolved in 50 ml of dry ethanol and the mixture was stirred at room temperature for 30 minutes under a nitrogen atmosphere. A solution of 4.000 g of the compound of (3) above in 30 ml of dry ethanol was added thereto and the mixture was refluxed for 15 hours. Methanol (50 ml) was added to the reaction mixture and the insoluble matters were removed. The solvent was distilled away under reduced pressure and the residue was purified by silica gel column chromatography to give 3.236 g of diethyl 2-acetamido-2-(2-pentadecynyl)malonate.

後処理

  1. temperaturethe mixture was refluxed for 15 hours
  2. customthe insoluble matters were removed
  3. distillationThe solvent was distilled away under reduced pressure
  4. customthe residue was purified by silica gel column chromatography

出典と根拠

ORDレコード
ord-d6deb23ebbca4508ab88028d7aea6871
出典データセット
uspto-grants-1998_02
特許番号
US05719176

反応ノート

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