Reaction #586148

Reaction equation

2-mercapto-4-(3-trifluoromethylpyrazolyl)benzonitrile

water

→

1,1′-thiodi-[2-cyano-5-(3-trifluoromethylpyrazolyl)benzene]

Yield 46.4%

Solvents

dimethyl sulfoxide

Conditions

Workup

1. 1
   Extractionthe organic matters were extracted with 20 ml of ethyl acetate twice
2. 2
   Washwashed with 30 ml of water twice
3. 3
   Dryingdried over anhydrous magnesium sulfate
4. 4
   workup.DISTILLATIONthe ethyl acetate was distilled off under reduced pressure
5. 5
   OtherPurification of the residue

Procedure

3.0 g (11.1 mmol) of 2-mercapto-4-(3-trifluoromethylpyrazolyl)benzonitrile in 5 ml of dimethyl sulfoxide was stirred at 50° C. for 2 hours. The reaction mixture was cooled to room temperature and poured into 50 ml of water, and the organic matters were extracted with 20 ml of ethyl acetate twice. The ethyl acetate layers were combined, then washed with 30 ml of water twice and dried over anhydrous magnesium sulfate, and the ethyl acetate was distilled off under reduced pressure. Purification of the residue afforded 1.3 g of 1,1′-thiodi-[2-cyano-5-(3-trifluoromethylpyrazolyl)benzene] (yield 42.4%) as a yellow solid, which was used in Example 2 (3) as the starting material.

Source