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Hydrochloric Acid → 2-Methylbenzophenone

HRID 1679249
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HRID 1679249 반응식
[C:1](Cl)(=[O:8])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[Cl-].[Al+3].[Cl-].[Cl-].O.Cl.[C:16]1([CH3:22])[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1>>[CH3:22][C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][C:17]=1[C:1]([C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1)=[O:8]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 5

HCID 313Hydrochloric AcidHCID 962WaterHCID 1140TolueneHCID 7412Benzoyl chlorideHCID 6451240Aluminum(III) Chloride

생성물 1

HCID 672302-Methylbenzophenone수율 93%

실험 절차

To a mechanically stirred solution of 1000 grams (7.12 moles) of benzoyl chloride in 6000 grams of toluene was added 1000 grams (7.50 moles) of anhydrous aluminum chloride over a 20- 30 minute period. The temperature of the reaction mixture rose to near the boiling point during the addition, and heating at reflux was maintained for three additional hours. After cooling, 1200 milliliters of water were added, slowly at first, followed by 1000 milliliters of concentrated hydrochloric acid. The organic layer was separated, washed twice with hot water and concentrated on a rotary evaporator. Vacuum distillation of the residual oil provided 1300 grams (93% yield) of white, semi-solid methyl benzophenone; (b.p. 180°-200° C., 10- 15 mm Hg; m.p. 50° C.) The infrared spectrum revealed a carbonyl band at 1665 cm -1.

후처리

  1. additionThe temperature of the reaction mixture rose to near the boiling point during the addition
  2. temperatureheating
  3. temperatureat reflux
  4. temperaturewas maintained for three additional hours
  5. temperatureAfter cooling
  6. customThe organic layer was separated
  7. washwashed twice with hot water
  8. concentrationconcentrated on a rotary evaporator
  9. distillationVacuum distillation of the residual oil

출처 및 근거

ORD 기록
ord-820b8d96fd9b4cbdbea9810f5e54b0f6
출처 데이터셋
uspto-grants-1978_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04080275

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