反応 #1543043

反応方程式

2-chloro-4-methylsulfonylbenzoyl chloride

aluminum chloride

1,1,2,2-tetrachloroethane

hydrochloric acid

→

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

反応条件

後処理

1. 1
   温度the mixture is subsequently refluxed for 7 hours
2. 2
   その他The organic phase is removed
3. 3
   抽出the aqueous phase is extracted twice
4. 4
   洗浄The combined organic phases are washed until neutral and
5. 5
   抽出subsequently extracted three times
6. 6
   ろ過The precipitate is filtered off
7. 7
   洗浄washed with water until neutral and
8. 8
   その他dried

実験手順

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.

出典