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

HRID 1200190ノート

反応式

HRID 1200190 の反応式
[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

参加物

5

反応物 3

HCID 887MethanolHCID 1118Sulfuric AcidHCID 14650449HCID 14650449、化合物

生成物 1

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

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

[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%.

後処理

  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

出典と根拠

ORDレコード
ord-dfd0c026e62f4617a5822473dc5ea50d
出典データセット
uspto-grants-1990_02
特許番号
US04904690

反応ノート

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