Ethanol → HCID 21281080, 화합물

HRID 414504

반응식

HRID 414504 반응식
[F:1][CH:2]([F:26])[C:3]([CH3:25])([CH3:24])[CH2:4][O:5][CH2:6][C:7]1[CH:12]=[CH:11][C:10]([F:13])=[C:9]([N:14]([C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=2)C(=O)C)[CH:8]=1.[OH-].[K+].C(O)C.C(OCC)(=O)C>O>[F:26][CH:2]([F:1])[C:3]([CH3:24])([CH3:25])[CH2:4][O:5][CH2:6][C:7]1[CH:12]=[CH:11][C:10]([F:13])=[C:9]([NH:14][C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=2)[CH:8]=1

참가 물질

6

반응물 4

HCID 702EthanolHCID 8857Ethyl AcetateHCID 14797Potassium HydroxideHCID 212810891,1-Difluoro-2,2-dimethyl-3-[3-(N-phenyl-N-acetylamino)-4-fluorobenzyloxy]propane

생성물 1

HCID 21281080HCID 21281080, 화합물수율 52%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

1,1-Difluoro-2,2-dimethyl-3-[3-(N-phenyl-N-acetylamino)-4fluorobenzyloxy]propane (0.5 g) was suspended in a 1 molar solution of potassium hydroxide in water containing 20% by volume ethanol and the mixture was heated at the reflux temperature for 8 hours. After standing overnight at the ambient temperature, the mixture was shaken several times with ethyl acetate and the combined organic extracts washed with water and brine, and dried over anhydrous magnesium sulphate. Evaporation of the solvent under reduced pressure gave a brown oil which was purified by column chromatography on a silica gel supoort, eluting with petroleum ether (boiling range 40°-60° C.) containing 10% by volume ethyl acetate, to give the title compound (0.23 g) as a pale yellow oil.

후처리

  1. temperaturethe mixture was heated at the reflux temperature for 8 hours
  2. washthe combined organic extracts washed with water and brine
  3. dry with materialdried over anhydrous magnesium sulphate
  4. customEvaporation of the solvent under reduced pressure
  5. customgave a brown oil which
  6. customwas purified by column chromatography on a silica gel supoort
  7. washeluting with petroleum ether (boiling range 40°-60° C.)
  8. additioncontaining 10% by volume ethyl acetate

출처 및 근거

ORD 기록
ord-a97baa1ff93c429eb52f47454fbbfa89
출처 데이터셋
uspto-grants-1988_12
특허 번호
US04792563

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