Methanol → Methyl [2-(1-cyclohexenyl)-4-oxo-4H-[1]-benzopyran-8-yl]acetate

HRID 1200190노트

반응식

HRID 1200190 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.[CH3:27]O>O>[C:1]1([C:7]2[O:8][C:9]3[C:17]([CH2:18][C:19]([O:21][CH3:27])=[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

5

반응물 3

HCID 887MethanolHCID 1118Sulfuric AcidHCID 14650449HCID 14650449, 화합물

생성물 1

HCID 14650461Methyl [2-(1-cyclohexenyl)-4-oxo-4H-[1]-benzopyran-8-yl]acetate수율 72%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

[2-(1-Cyclohexenyl)-4-oxo-4H-[1]-benzopyran-8-yl]acetic acid (1.42 g) and conc. sulfuric acid (0.2 ml) were dded to methanol (30 ml) and the mixture was refluxed for 3 hours. Then, water was added. The mixture was extracted with ethyl acetate and the extracted layer was washed and dried. Ethyl acetate was distilled off under reduced pressure and the residue was recrystallized from hexane-ethyl acetate to obtain the title compound, m.p. 137°-138° C., yield 72%.

후처리

  1. temperaturethe mixture was refluxed for 3 hours
  2. extractionThe mixture was extracted with ethyl acetate
  3. washthe extracted layer was washed
  4. customdried
  5. distillationEthyl acetate was distilled off under reduced pressure
  6. customthe residue was recrystallized from hexane-ethyl acetate

출처 및 근거

ORD 기록
ord-dfd0c026e62f4617a5822473dc5ea50d
출처 데이터셋
uspto-grants-1990_02
특허 번호
US04904690

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