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

HRID 488333노트

반응식

HRID 488333 반응식
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]

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

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

후처리

  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

출처 및 근거

ORD 기록
ord-01ad4cc0a4c64417abd899ac46606e88
출처 데이터셋
uspto-grants-1994_03
특허 번호
US05298652

반응 노트

불러오는 중…