4-Chloro-o-xylene → 2,2'-Dichloro-4,4',5,5'-tetramethylbenzophenone

HRID 255470

반응식

HRID 255470 반응식
[Al+3].[Cl-:2].[Cl-:3].[Cl-].Cl[C:6]1[CH:7]=[C:8]([CH3:13])[C:9]([CH3:12])=[CH:10][CH:11]=1.[C:14](Cl)(=[O:18])[C:15](Cl)=O>C(=S)=S>[Cl:2][C:11]1[CH:10]=[C:9]([CH3:12])[C:8]([CH3:13])=[CH:7][C:6]=1[C:14]([C:15]1[CH:10]=[C:9]([CH3:12])[C:8]([CH3:13])=[CH:7][C:6]=1[Cl:3])=[O:18]

참가 물질

5

반응물 3

HCID 328864-Chloro-o-xyleneHCID 65578Oxalyl chlorideHCID 6451240Aluminum(III) Chloride

생성물 1

HCID 150271722,2'-Dichloro-4,4',5,5'-tetramethylbenzophenone수율 67.9%

시약·촉매·용매 1

HCID 6348Carbon Disulfide용매

실험 절차

146 g of AlCl3 are added to a solution of 140 g of 4-chloro-o-xylene and 68 g of oxalyl chloride in 500 ml of CS2 at 0°-5°C. in the course of 2 hours, with stirring. After 20 hours, the mixture is poured onto ice and extracted with 600 ml of CHCl3. The extract is washed with water, dried and evaporated completely. Recrystallisation of the residue from diisopropyl ether gives 103.8 g of 2,2'-dichloro-4,4',5,5'-tetramethylbenzophenone (D). Melting point: 148°-149° C.

후처리

  1. additionthe mixture is poured onto ice
  2. extractionextracted with 600 ml of CHCl3
  3. washThe extract is washed with water
  4. customdried
  5. customevaporated completely
  6. customRecrystallisation of the residue from diisopropyl ether

출처 및 근거

ORD 기록
ord-a1700d5b417a47799cf30df7de44a2e5
출처 데이터셋
uspto-grants-1987_10
특허 번호
US04698295

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