Ethanol → HCID 14650456, 화합물

HRID 1200188노트

반응식

HRID 1200188 반응식
[C:1]1([C:7]2[O:8][C:9]3[C:17]([CH2:18][C:19]([OH:21])=[O:20])=[CH:16][CH:15]=[CH:14][C:10]=3[C:11](=[O:13])[CH:12]=2)[CH2:6][CH2:5][CH2:4][CH2:3][CH:2]=1.S(=O)(=O)(O)O.[CH2:27](O)[CH3:28]>>[C:1]1([C:7]2[O:8][C:9]3[C:17]([CH2:18][C:19]([O:21][CH2:27][CH3:28])=[O:20])=[CH:16][CH:15]=[CH:14][C:10]=3[C:11](=[O:13])[CH:12]=2)[CH2:6][CH2:5][CH2:4][CH2:3][CH:2]=1

참가 물질

4

반응물 3

HCID 702EthanolHCID 1118Sulfuric AcidHCID 14650449HCID 14650449, 화합물

생성물 1

HCID 14650456HCID 14650456, 화합물

실험 절차

[2-(1-Cyclohexenyl)-4-oxo-4H-[1]-benzopyran-8-yl]acetic acid (2.0 g) was dissolved in ethanol (50 ml) and to the solution was added conc. sulfuric acid (0.5 ml). The mixture was heated under reflux for 5 hours. After dilution with water, the mixture was extracted with ethyl acetate and the extract was washed with water, dried (MgSO4) and concentrated under reduced pressure to obtain the title compound as crystals. The crystals were recrystallized from ethyl acetate to obtain prisms, yield 1.34 g (61.0%), m.p. 126°-127° C.

후처리

  1. temperatureThe mixture was heated
  2. temperatureunder reflux for 5 hours
  3. extractionAfter dilution with water, the mixture was extracted with ethyl acetate
  4. washthe extract was washed with water
  5. dry with materialdried (MgSO4)
  6. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-90bb2b0bde91408a8b1e5f90916d1703
출처 데이터셋
uspto-grants-1990_02
특허 번호
US04904690

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