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Aluminum(III) Chloride → HCID 23303967, 화합물

HRID 1421415
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HRID 1421415 반응식
[Cl:1][C:2]1[C:3]([F:13])=[C:4]([C:9](F)(F)F)[CH:5]=[CH:6][C:7]=1[F:8].[Al+3].[Cl-:15].[Cl-:16].[Cl-:17]>C(Cl)Cl>[Cl:1][C:2]1[C:3]([F:13])=[C:4]([C:9]([Cl:17])([Cl:16])[Cl:15])[CH:5]=[CH:6][C:7]=1[F:8]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 6451240Aluminum(III) ChlorideHCID 143926222-Chloro-1,3-difluoro-4-(trifluoromethyl)benzene

생성물 1

HCID 23303967HCID 23303967, 화합물수율 86.9%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

반응 조건

온도
42 °C

실험 절차

216.5 g of 3-chloro-2,4-difluoro-benzotrifluoride in 440 ml of methylene chloride are initially introduced into a stirred apparatus, and 150 g of AlCl3 are introduced in small portions. The reaction is slightly exothermic. When the addition has ended, the mixture is heated under reflux (42° C.) for 2 hours, cooled and poured onto 1 l of ice-water. After intensive thorough mixing, the mixture is filtered over a suction filter and the organic phase is then separated off. After drying, the methylene chloride phase is distilled. 231 g of 3-chloro-2,4-difluoro-benzotrichloride with a boiling range of 124-126° C./18 mbar are obtained.

후처리

  1. additionare introduced in small portions
  2. additionWhen the addition
  3. temperaturethe mixture is heated
  4. temperaturecooled
  5. filtrationAfter intensive thorough mixing, the mixture is filtered over a suction
  6. filtrationfilter
  7. customthe organic phase is then separated off
  8. customAfter drying
  9. distillationthe methylene chloride phase is distilled

출처 및 근거

ORD 기록
ord-ada5d7286781454aa1537b3e74514479
출처 데이터셋
uspto-grants-2000_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06075165

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