Diethyl methyl(4-nitrophenyl)propanedioate → HCID 12370795、化合物

HRID 2176906ノート

反応式

HRID 2176906 の反応式
[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

参加物

3

反応物 1

HCID 12380744Diethyl methyl(4-nitrophenyl)propanedioate

生成物 1

HCID 12370795HCID 12370795、化合物収率 83.5%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-d9819b59497d46278559ad443ff7e996
出典データセット
uspto-grants-2015_06
特許番号
US09067888B2

反応ノート

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