Hydrochloric Acid → 2,3-Dichloro-4-methoxy-4'-chloro-2'-fluorobenzophenone

HRID 652920

반응식

HRID 652920 반응식
[Cl:1][C:2]1[CH:10]=[CH:9][C:5]([C:6](Cl)=[O:7])=[C:4]([F:11])[CH:3]=1.[Cl:12][C:13]1[C:18]([Cl:19])=[CH:17][CH:16]=[CH:15][C:14]=1[O:20][CH3:21].[Al+3].[Cl-].[Cl-].[Cl-].Cl>ClCCCl>[Cl:19][C:18]1[C:13]([Cl:12])=[C:14]([O:20][CH3:21])[CH:15]=[CH:16][C:17]=1[C:6]([C:5]1[CH:9]=[CH:10][C:2]([Cl:1])=[CH:3][C:4]=1[F:11])=[O:7]

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 161262,3-DichloroanisoleHCID 27736014-Chloro-2-fluorobenzoyl chlorideHCID 6451240Aluminum(III) Chloride

생성물 1

HCID 140972672,3-Dichloro-4-methoxy-4'-chloro-2'-fluorobenzophenone

시약·촉매·용매 1

HCID 111,2-Dichloroethane용매

반응 조건

온도
40 °C

실험 절차

To a mixture of 46 g of 4-chloro-2-fluorobenzoyl chloride and 38.9 g of 2,3-dichloroanisole in 150 ml of 1,2-dichloroethane, 32 g of AlCl3 is added gradually. The mixture is warmed to 40° C. with a vigorous evolution of gas. The mixture is poured into concentrated HCl and ice. The organic layer is separated and the aqueous layer is extracted with additional organic solvent. The combined organic extracts are washed with water, dried over Na2SO4 and evaporated. The crude product is triturated with hexane to give 2,3-dichloro-4-methoxy-4'-chloro-2'-fluorobenzophenone. An analytical sample is recrystallized from EtOH, mp 115°-116° C.

후처리

  1. additionis added gradually
  2. customThe organic layer is separated
  3. extractionthe aqueous layer is extracted with additional organic solvent
  4. washThe combined organic extracts are washed with water
  5. dry with materialdried over Na2SO4
  6. customevaporated
  7. customThe crude product is triturated with hexane

출처 및 근거

ORD 기록
ord-065ee68acb964175a273abc4b4654929
출처 데이터셋
uspto-grants-1987_06
특허 번호
US04673746

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