Water → Diethyl 2-Amino-2-(4-Octylphenethyl)malonate

HRID 1451615ノート

反応式

HRID 1451615 の反応式
[H-].[Na+].[CH2:3]([O:5][C:6]([CH:8]([CH2:14][CH2:15][C:16]1[CH:21]=[CH:20][C:19]([CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH3:29])=[CH:18][CH:17]=1)[C:9]([O:11][CH2:12][CH3:13])=[O:10])=[O:7])[CH3:4].[N+:30](C1C=C([N+]([O-])=O)C=CC=1ON)([O-])=O.O>CN(C)C=O>[NH2:30][C:8]([C:9]([O:11][CH2:12][CH3:13])=[O:10])([CH2:14][CH2:15][C:16]1[CH:17]=[CH:18][C:19]([CH2:22][CH2:23][CH2:24][CH2:25][CH2:26][CH2:27][CH2:28][CH3:29])=[CH:20][CH:21]=1)[C:6]([O:5][CH2:3][CH3:4])=[O:7]

参加物

6

反応物 4

HCID 962WaterHCID 24758Sodium hydrideHCID 87140O-(2,4-dinitrophenyl)hydroxylamineHCID 21849265Ethyl 2-Ethoxycarbonyl-4-(4-octylphenyl)butyrate

生成物 1

HCID 21849165Diethyl 2-Amino-2-(4-Octylphenethyl)malonate収率 133.8%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

60% Sodium hydride (0.38 g) was suspended in dry dimethylformamide (30 ml) and ethyl 2-ethoxycarbonyl-4-(4-octylphenyl)butyrate (3.0 g) was added thereto. The mixture was stirred at room temperature for 2 hours. O-(2,4-Dinitrophenyl)hydroxylamine (1.14 g) was added thereto and the mixture was stirred at room temperature for 5 hours. The reaction mixture was poured into cool water and extracted with toluene. The extract was washed with aqueous sodium chloride and dried over magnesium sulfate. The solvent was distilled away under reduced pressure to give 3 g of the subject compound.

後処理

  1. stirringthe mixture was stirred at room temperature for 5 hours
  2. additionThe reaction mixture was poured
  3. extractionextracted with toluene
  4. washThe extract was washed with aqueous sodium chloride
  5. dry with materialdried over magnesium sulfate
  6. distillationThe solvent was distilled away under reduced pressure

出典と根拠

ORDレコード
ord-4c5a4ba4e05c4189a6e39aff756ad609
出典データセット
uspto-grants-1997_02
特許番号
US05604229

反応ノート

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