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Hydrochloric Acid → 5-Ethyl-2-methoxy-4'-trifluoromethylbenzophenone

HRID 1391338
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HRID 1391338 반응식
[Cl-].[Al+3].[Cl-].[Cl-].[F:5][C:6]([F:17])([F:16])[C:7]1[CH:15]=[CH:14][C:10]([C:11](Cl)=[O:12])=[CH:9][CH:8]=1.[CH2:18]([C:20]1[CH:25]=[CH:24][C:23]([O:26][CH3:27])=[CH:22][CH:21]=1)[CH3:19].Cl>ClCCl>[CH2:18]([C:20]1[CH:21]=[CH:22][C:23]([O:26][CH3:27])=[C:24]([CH:25]=1)[C:11]([C:10]1[CH:14]=[CH:15][C:7]([C:6]([F:17])([F:16])[F:5])=[CH:8][CH:9]=1)=[O:12])[CH3:19]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 676074-(Trifluoromethyl)benzoyl chlorideHCID 736901-Ethyl-4-methoxybenzeneHCID 6451240Aluminum(III) Chloride

생성물 1

HCID 213309645-Ethyl-2-methoxy-4'-trifluoromethylbenzophenone수율 88.5%

시약·촉매·용매 1

HCID 6344
Dichloromethane
용매
2회

실험 절차

Aluminium chloride (0.6 g, 0.004 mole) was stirred in dichloromethane (2 ml) and treated with 4-trifluoromethylbenzoyl chloride (1 g, 0.0048 mole) (ice-bath cooling) and then with 4-ethylanisole (0.6 g, 0.0044 mole) in dichloromethane (1 ml). The mixture was stirred at room temperature overnight and then poured into ice and concentrated hydrochloric acid and extracted with chloroform. The chloroform solution was washed with 10% NaHCO3 solution (100 ml), dried (MgSO4), filtered and evaporated to leave 5-ethyl-2-methoxy-4'-trifluoromethylbenzophenone (1.2 g) as a yellow oil. The latter was heated in 55% aqueous hydrogen bromide (27.5 ml) at 110°-120° C. for 5 hours. The mixture was evaporated to dryness to leave the required product.

후처리

  1. extractionextracted with chloroform
  2. washThe chloroform solution was washed with 10% NaHCO3 solution (100 ml)
  3. dry with materialdried (MgSO4)
  4. filtrationfiltered
  5. customevaporated

출처 및 근거

ORD 기록
ord-19b9f76e796a4b278719148d0a15ce32
출처 데이터셋
uspto-grants-1979_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04141995

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