Preparation method of 2-(3, 3, 3-trifluoro propyl) benzsulfamide (I) and midbody thereof
A technology of trifluoropropanyl and benzenesulfonamide, which is applied in the preparation of sulfonamides and organic chemistry, etc., can solve the problems of difficult industrial operation, high price, and high synthesis cost, and achieve the effect of simple industrial operation and low cost
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Embodiment 1
[0030] Example 1 Synthesis method of 4,5-dichloro-2-(3,3,3-trifluoropropanyl)benzenesulfonamide (II).
[0031] Add 5.7ml of chlorosulfonic acid to the flask, and cool it to 0°C with ice salt; add 5.0g (0.029mol) of 1,2-dichloro-4-(3,3,3-trifluoropropyl)benzene dropwise, and control the temperature At less than 50°C, the addition was completed in about 1 hour; at 0-5°C for 4 hours, the reaction solution turned into a yellow-brown viscous oil; put 20g of ice and 5ml of ice water in an ice bath; pour the reaction solution slowly Pour into ice water, keep stirring while controlling the temperature to less than 10-15°C; precipitate a white solid, cool for 15 minutes, and filter with suction to obtain the product (MS: 340); add 10ml of dichloroethane, stir to dissolve, cool to 0°C, add dropwise excess Ammonia water, the temperature of the reaction solution is less than 40°C; after dropping, reach room temperature, pH = 8-9; filter with suction and wash with water to obtain the white...
Embodiment 2
[0032] Example 2 Synthesis of 4,5-dichloro-2-(3,3,3-trifluoropropane)benzenesulfonamide (II).
[0033] Add 5.7ml of chlorosulfonic acid to the flask, and cool it to 0°C with ice salt; add 5.0g (0.029mol) of 1,2-dichloro-4-(3,3,3-trifluoropropyl)benzene dropwise, and control the temperature At less than 10°C, the addition was completed in about 1 hour; when the temperature was raised to room temperature, the reaction solution turned into a yellow-brown viscous oil; the reaction was stirred for 5 hours, and 20 g of ice and 5 ml of ice water were placed in an ice bath; the reaction solution was poured slowly Pour into ice water, keep stirring while controlling the temperature to less than 10-15°C; precipitate a white solid, cool for 15 minutes, and filter with suction to obtain the product (MS: 340); add 10ml of dichloroethane, stir to dissolve, cool to 0°C, add dropwise excess Ammonia water, the temperature of the reaction solution is less than 40°C; after dropping, reach room t...
Embodiment 3
[0034] Example 3 Synthesis of 4,5-dichloro-2-(3,3,3-trifluoropropane)benzenesulfonamide (II).
[0035] Add 5.7ml of chlorosulfonic acid to the flask, and cool it to 0°C with ice salt; add 5.0g (0.029mol) of 1,2-dichloro-4-(3,3,3-trifluoropropyl)benzene dropwise, and control the temperature At less than 10°C, the addition was completed in about 1 hour; warmed up to room temperature, and heated in a water bath to 55°C for 4 hours, the reaction solution turned into a yellow-brown viscous oil; put 20g of ice and 5ml of ice water in an ice bath; put the reaction The solution was slowly poured into ice water, and the temperature was controlled to be less than 10-15°C while stirring; a white solid was precipitated, cooled for 15 minutes, and the product (MS: 340) was obtained by suction filtration; 10ml of dichloroethane was added, stirred and dissolved, and then cooled to 0°C. Through the amount of ammonia gas, the temperature of the reaction solution is less than 40°C; after droppi...
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