Water → alpha-Oxo-4-[(12-phenoxydodecyl)oxy]benzeneacetic acid

HRID 488333ノート

反応式

HRID 488333 の反応式
C([O:3][C:4](=[O:33])[C:5](=[O:32])[C:6]1[CH:11]=[CH:10][C:9]([O:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][O:25][C:26]2[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=2)=[CH:8][CH:7]=1)C.[OH-].[Na+].O>CO>[O:32]=[C:5]([C:6]1[CH:11]=[CH:10][C:9]([O:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][O:25][C:26]2[CH:27]=[CH:28][CH:29]=[CH:30][CH:31]=2)=[CH:8][CH:7]=1)[C:4]([OH:33])=[O:3]

参加物

5

反応物 3

HCID 962WaterHCID 14798Sodium HydroxideHCID 54340854alpha-Oxo-4-[(12-phenoxydodecyl)oxy]benzeneacetic acid ethyl ester

生成物 1

HCID 19091785alpha-Oxo-4-[(12-phenoxydodecyl)oxy]benzeneacetic acid収率 84.3%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

To 1.44 g (3.17 mmol) of alpha-oxo-4-[(12-phenoxydodecyl)oxy]benzeneacetic acid ethyl ester in 100 ml of hot methanol was added 3.5 ml (3.5 mmol) of 1N NaOH. The mixture was heated on a steam bath for 5 minutes, water (20 ml) was added and the solvents were removed at reduced pressure. Water (100 ml) and 7.0 ml of 1.0N HCl were added to the residue and the product was extracted with methylene chloride-THF (4:1). The dried extract was concentrated at reduced pressure to a solid which was recrystallized from acetone-hexane to give 1.14 g (84% yield, mp 98°-100°) of alpha-oxo-4-[(12-phenoxydodecyl)oxy]benzeneacetic acid

後処理

  1. temperatureThe mixture was heated on a steam bath for 5 minutes
  2. customthe solvents were removed at reduced pressure
  3. additionWater (100 ml) and 7.0 ml of 1.0N HCl were added to the residue
  4. extractionthe product was extracted with methylene chloride-THF (4:1)
  5. extractionThe dried extract
  6. concentrationwas concentrated at reduced pressure to a solid which
  7. customwas recrystallized from acetone-hexane

出典と根拠

ORDレコード
ord-01ad4cc0a4c64417abd899ac46606e88
出典データセット
uspto-grants-1994_03
特許番号
US05298652

反応ノート

読み込み中…