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

HRID 862853노트

반응식

HRID 862853 반응식
[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]

참가 물질

6

반응물 4

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

생성물 1

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

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-73664319c1ca4297a83908be44456183
출처 데이터셋
uspto-grants-1998_02
특허 번호
US05719176

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