Benzene → 1,6-Diphenyl-1,6-hexanedione

HRID 1377220노트

반응식

HRID 1377220 반응식
[Cl-].[Al+3].[Cl-].[Cl-].[C:5](Cl)(=[O:13])[CH2:6][CH2:7][CH2:8][CH2:9][C:10](Cl)=[O:11].[CH:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1>>[C:15]1([C:5](=[O:13])[CH2:6][CH2:7][CH2:8][CH2:9][C:10]([C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=2)=[O:11])[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1

참가 물질

4

반응물 3

HCID 241Benzene2회HCID 61034Adipoyl chlorideHCID 6451240Aluminum(III) Chloride

생성물 1

HCID 769031,6-Diphenyl-1,6-hexanedione

실험 절차

In a 2-liter three-necked flask equipped with a stirring device, a thermometer and a nitrogen substituting device, 700 milliliters of benzene was introduced and 177.0 g of aluminum chloride was added with ice cooling. Then, a solution of 101.6 g of adipoyl chloride in 300 milliliters of benzene was added dropwise for 35 minutes. After stirring for one day and one night with warming back to the room temperature, the solution was poured in 3 liters of ice water containing dilute hydrochloric acid, and extracted with 2.5 liters of toluene. Thereafter, the solution was washed with a 0.5N aqueous solution of sodium hydroxide and water, and then dried with anhydrous magnesium sulfate. After removing off the solvent by a rotary evaporator, 128.4 g of 1,6-diphenylhexane-1,6-dione was obtained as crystals by recrystallizing the obtained crystals from ethyl acetate.

후처리

  1. customIn a 2-liter three-necked flask equipped with a stirring device
  2. extractionextracted with 2.5 liters of toluene
  3. washThereafter, the solution was washed with a 0.5N aqueous solution of sodium hydroxide and water
  4. dry with materialdried with anhydrous magnesium sulfate
  5. customAfter removing off the solvent
  6. customby a rotary evaporator

출처 및 근거

ORD 기록
ord-054ecf1c5ed241dabb0e76861f2a6182
출처 데이터셋
uspto-grants-1997_09
특허 번호
US05663440

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