Ethanol → HCID 14650456, 화합물

HRID 1200195노트

반응식

HRID 1200195 반응식
Br[C:2]1([C:8]2[O:9][C:10]3[C:18]([CH2:19][C:20]#N)=[CH:17][CH:16]=[CH:15][C:11]=3[C:12](=[O:14])[CH:13]=2)[CH2:7][CH2:6][CH2:5][CH2:4][CH2:3]1.S(=O)(=O)(O)[OH:23].[CH2:27]([OH:29])[CH3:28]>>[C:2]1([C:8]2[O:9][C:10]3[C:18]([CH2:19][C:20]([O:29][CH2:27][CH3:28])=[O:23])=[CH:17][CH:16]=[CH:15][C:11]=3[C:12](=[O:14])[CH:13]=2)[CH2:7][CH2:6][CH2:5][CH2:4][CH:3]=1

참가 물질

4

반응물 3

HCID 702EthanolHCID 1118Sulfuric AcidHCID 146504442-(1-Bromocyclohexyl)-8-cyanomethyl-4-oxo-4H-[1]-benzopyran

생성물 1

HCID 14650456HCID 14650456, 화합물수율 56%

실험 절차

2-(1-Bromocyclohexyl)-8-cyanomethyl-4-oxo-4H-[1]-benzopyran (5.0 g) and 50% sulfuric acid (4 ml) were added to ethanol (400 ml) and the mixture was refluxed for 8 hours. Then, ethanol (about 300 ml) was distilled off under reduced pressure and the residue was added to water. The mixture was extracted with ethyl acetate and the extract was washed with water, dried (MgSO4) and concentrated. The residue was recrystallized from ethyl acetate to obtain the title compound, yield 56%.

후처리

  1. temperaturethe mixture was refluxed for 8 hours
  2. distillationThen, ethanol (about 300 ml) was distilled off under reduced pressure
  3. additionthe residue was added to water
  4. extractionThe mixture was extracted with ethyl acetate
  5. washthe extract was washed with water
  6. dry with materialdried (MgSO4)
  7. concentrationconcentrated
  8. customThe residue was recrystallized from ethyl acetate

출처 및 근거

ORD 기록
ord-91715fe907ea4772961b884df4ebe04a
출처 데이터셋
uspto-grants-1990_02
특허 번호
US04904690

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