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ChemicalBook CAS DataBase List 4-Chloro-2-fluorobenzenethiol
73129-12-1

4-Chloro-2-fluorobenzenethiol synthesis

3synthesis methods
-

Yield:73129-12-1 25%

Reaction Conditions:

with triphenylphosphine in toluene at 20; for 0.5 h;

Steps:

103.1 Step 1: 2-fluoro-4-chlorobenzenethiol

To a stirred solution of 2-fluoro-4-chlorobenzenesulfonyl chloride (460 mg, 2.0 mmol) in toluene (12 mL) was added triphenylphosphine (1.6 g, 6.0 mmol), the mixture was stirred at RT for 30 mins. TLC showed the reaction was complete. Water (5 mL) was added and the mixture was stirred for 10 mins, aqueous layer was discarded and organic layer was extracted with 10% of sodium hydroxide solution (30 mL), the aqueous layer was washed with toluene (20 mL), acidified with 2N hydrochloric acid and extracted with DCM (30 mL). The combined organic layers were dried over sodium sulfate and concentrated under reduced pressure to afford the product of 2-fluoro-4-chlorobenzenethiol (80 mg, 25%) as a yellow oil, which was used in next step without further purification.

References:

WO2022/140464,2022,A1 Location in patent:Page/Page column 62