Acetone → 2,2-Dimethyl-chroman-4-one

HRID 247852

反応式

HRID 247852 の反応式
O[CH2:2][C:3]([C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1)=[O:4].[CH3:11][C:12]([CH3:14])=[O:13].N1CCCC1>C1(C)C=CC=CC=1>[CH3:11][C:12]1([CH3:14])[O:13][C:10]2[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=2[C:3](=[O:4])[CH2:2]1

参加物

5

反応物 3

HCID 180AcetoneHCID 31268PyrrolidineHCID 68490alpha-Hydroxyacetophenone

生成物 1

HCID 74542902,2-Dimethyl-chroman-4-one収率 21.6%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

Twenty five grams (25 g) of 2-hydroxyacetophenon, 10.7 g of acetone, and 5.5 g of pyrrolidine were added to 50 ml of toluene, and heated and refluxed. Twenty hours later, the temperature was returned to ambient temperature and the solvent was distilled off under reduced pressure, to which was added 100 ml of 1N hydrogen chloride. The extraction was carried out with 50 ml×3 of chloroform, followed by washing in water, drying over anhydrous magnesium sulfate, filtering off and condensation of the filtered solution. The residue was purified on a silica gel column the fraction containing the purified product were mixed together and the solvent therein was distilled off under reduced pressure to obtain 7 g of 3,4-dihydro-2,2-dimethyl-2H-benzo[b]pyran-4-one.

後処理

  1. temperatureheated
  2. temperaturerefluxed
  3. customTwenty hours
  4. customwas returned to ambient temperature
  5. distillationthe solvent was distilled off under reduced pressure, to which
  6. additionwas added 100 ml of 1N hydrogen chloride
  7. extractionThe extraction
  8. washby washing in water
  9. dry with materialdrying over anhydrous magnesium sulfate
  10. filtrationfiltering off
  11. customcondensation of the filtered solution
  12. customThe residue was purified on a silica gel column the fraction
  13. additioncontaining the purified product
  14. additionwere mixed together
  15. distillationthe solvent therein was distilled off under reduced pressure

出典と根拠

ORDレコード
ord-fabe6bcff6424db1a3d54fe34d9c4a15
出典データセット
uspto-grants-1993_05
特許番号
US05208245

関連ノート

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