Diethyl methyl(4-nitrophenyl)propanedioate → HCID 12370795, 화합물

HRID 2176906노트

반응식

HRID 2176906 반응식
[CH3:1][C:2]([C:13]1[CH:18]=[CH:17][C:16]([N+:19]([O-])=O)=[CH:15][CH:14]=1)([C:8]([O:10][CH2:11][CH3:12])=[O:9])[C:3]([O:5][CH2:6][CH3:7])=[O:4]>CCO>[NH2:19][C:16]1[CH:17]=[CH:18][C:13]([C:2]([CH3:1])([C:3]([O:5][CH2:6][CH3:7])=[O:4])[C:8]([O:10][CH2:11][CH3:12])=[O:9])=[CH:14][CH:15]=1

참가 물질

3

반응물 1

HCID 12380744Diethyl methyl(4-nitrophenyl)propanedioate

생성물 1

HCID 12370795HCID 12370795, 화합물수율 83.5%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

Stannous chloride dihydrate (30.60 g, 135.6 mmol) was added to a solution of diethyl 2-methyl-2-(4-nitrophenyl)malonate (8.00 g, 27.1 mmol) in EtOH (100 ml) and stirred at reflux for 16 h. The reaction mixture was cooled to room temperature and concentrated under reduced pressure. The residue was taken in water and basified with triethyl amine to adjust a pH˜8. The precipitated solid was filtered and washed with ethyl acetate. The separated organic layer from the filtrate was washed with water, brine solution, dried over anhydrous sodium sulfate, filtered and concentrated under reduced pressure to afford 6.0 g (83%) of diethyl 2-(4-aminophenyl)-2-methylmalonate as brown oil.

후처리

  1. temperatureat reflux for 16 h
  2. concentrationconcentrated under reduced pressure
  3. filtrationThe precipitated solid was filtered
  4. washwashed with ethyl acetate
  5. washThe separated organic layer from the filtrate was washed with water, brine solution
  6. dry with materialdried over anhydrous sodium sulfate
  7. filtrationfiltered
  8. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-d9819b59497d46278559ad443ff7e996
출처 데이터셋
uspto-grants-2015_06
특허 번호
US09067888B2

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