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

HRID 35154

反応式

HRID 35154 の反応式
[Na].[C:2]([NH:5][CH:6]([C:12]([O:14][CH2:15][CH3:16])=[O:13])[C:7]([O:9][CH2:10][CH3:11])=[O:8])(=[O:4])[CH3:3].[C:17]1([CH:23]([C:25]2[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=2)Br)[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1>C(O)C>[C:2]([NH:5][C:6]([CH:23]([C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1)[C:25]1[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=1)([C:12]([O:14][CH2:15][CH3:16])=[O:13])[C:7]([O:9][CH2:10][CH3:11])=[O:8])(=[O:4])[CH3:3]

参加物

5

反応物 3

HCID 14041Acetamidomalonic acid diethyl esterHCID 236603BromodiphenylmethaneHCID 5360545Sodium

生成物 1

HCID 14211495Diethyl 2-acetamido-2-(diphenylmethyl)malonate

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

Dissolve sodium (2 g) in 400 ml ethanol and add diethyl acetamidomalonate (10.4 g). Stir 5 minutes, add diphenyl bromomethane (12.4 g), and stir 7 hours at room temperature. Acidify the reaction mixture, partition between water and methylene chloride (CH2Cl2), dry the organic layer over magnesium sulfate (MgSO4), filter, and evaporate the solvent to obtain the crude title compound as a pale yellow oil. Rf (silica gel; Et2O)=0.89.

後処理

  1. stirringstir 7 hours at room temperature
  2. custompartition between water and methylene chloride (CH2Cl2)
  3. dry with materialdry the organic layer over magnesium sulfate (MgSO4)
  4. filtrationfilter
  5. customevaporate the solvent

出典と根拠

ORDレコード
ord-18b2b873df424d9bacf447d4ae203cba
出典データセット
uspto-grants-1988_08
特許番号
US04766109

関連ノート

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