Реакция #1543043

Уравнение реакции

2-chloro-4-methylsulfonylbenzoyl chloride

aluminum chloride

1,1,2,2-tetrachloroethane

hydrochloric acid

→

2,2', 4'-Trichloro-6'-hydroxy-4-methylsulfonylbenzophenone

Условия реакции

Обработка

1. 1
   Температураthe mixture is subsequently refluxed for 7 hours
2. 2
   ДругоеThe organic phase is removed
3. 3
   Экстракцияthe aqueous phase is extracted twice
4. 4
   ПромывкаThe combined organic phases are washed until neutral and
5. 5
   Экстракцияsubsequently extracted three times
6. 6
   ФильтрацияThe precipitate is filtered off
7. 7
   Промывкаwashed with water until neutral and
8. 8
   Другоеdried

Методика

3.00 g of 2-chloro-4-methylsulfonylbenzoyl chloride are added in portions at room temperature to a mixture of 1.97 g of 3,5-dichlorophenone and 3.23 g of aluminum chloride in 50 ml of 1,1,2,2-tetrachloroethane, and the mixture is subsequently refluxed for 7 hours. When cold, the reaction mixture is poured onto 100 g of ice and 20 ml of concentrated hydrochloric acid. The organic phase is removed, and the aqueous phase is extracted twice using 50 ml of dichloromethane. The combined organic phases are washed until neutral and subsequently extracted three times using in each case 25 ml of 2N sodium hydroxide solution. The combined alkaline extracts are brought to a pH of 2 using concentrated hydrochloric acid. The precipitate is filtered off, washed with water until neutral and dried. This gives 3.194 g (70% of theory) of 2,2', 4'-trichloro-6'-hydroxy-4-methylsulfonylbenzophenone in the form of colorless crystals with a melting point of 123°-126° C.

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