Ethanol → HCID 14650456、化合物

HRID 1200195ノート

反応式

HRID 1200195 の反応式
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

参加物

4

反応物 3

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

生成物 1

HCID 14650456HCID 14650456、化合物収率 56%

実験手順

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%.

後処理

  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

出典と根拠

ORDレコード
ord-91715fe907ea4772961b884df4ebe04a
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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