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

HRID 255470

反応式

HRID 255470 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

HCID 150271722,2'-Dichloro-4,4',5,5'-tetramethylbenzophenone収率 67.9%

試薬・触媒・溶媒 1

HCID 6348Carbon Disulfide溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-a1700d5b417a47799cf30df7de44a2e5
出典データセット
uspto-grants-1987_10
特許番号
US04698295

関連ノート

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