A 3-sulfonyl-5-difluoromethyl phosphate modified pyrazoline derivative and preparation method thereof
A technology of difluoromethyl phosphate and pyrazoline, applied in the field of pyrazoline derivatives and their preparation, can solve the problems of low total yield, numerous reaction steps, difficult to control functional group sites and the like
- Summary
- Abstract
- Description
- Claims
- Application Information
AI Technical Summary
Problems solved by technology
Method used
Image
Examples
Embodiment 1
[0036] Weigh 50 mmol of the amine compound (Ar 1 =C 6 H 5 ) was dissolved in 50mL carbon tetrachloride, successively added tert-butyl nitrite 50mmol, acetic acid 25mmol, heated to 60 ℃, reacted for 20 minutes, then cooled to room temperature, then added 25mmol vinyl sulfone compound ( Ar 2 =C 6 H 5 ), and the reaction was stirred at room temperature for 16 hours. After the reaction finishes, remove the solvent under reduced pressure to obtain the crude product, then separate and purify the target product with column chromatography (petroleum ether and ethyl acetate as eluent, with a volume ratio of 4:1) to obtain the target product. Figure 1-4 As shown, the yield was 58%.
Embodiment 2
[0038] Weigh 25 mmol of the amine compound (Ar 1 =C 6 H 5 ) was dissolved in 30 mL of tetrahydrofuran, successively added 30 mmol of t-butyl nitrite and 10 mmol of acetic acid, heated to 60 ° C, reacted for 20 minutes, then cooled to room temperature, and then added 25 mmol of vinyl sulfone compounds (Ar 2 =C 6 H 5 ), and the reaction was stirred at room temperature for 16 hours. After the reaction, remove the solvent under reduced pressure to obtain the crude product, and then separate and purify the target product with column chromatography (petroleum ether and ethyl acetate as eluent, with a volume ratio of 4:1) to obtain the target product. 1 was consistent and was not provided in duplicate in 41% yield.
Embodiment 3
[0040] Weigh 75 mmol of the amine compound (Ar 1 =C 6 H 5 ) was dissolved in 60 mL of carbon tetrachloride, successively added 90 mmol of tert-butyl nitrite, 35 mmol of acetic acid, heated to 60 ° C, reacted for 20 minutes, then cooled to room temperature, then added 25 mmol of vinyl sulfone compounds ( Ar 2 =C 6 H 5 ), and the reaction was stirred at room temperature for 16 hours. After the reaction, remove the solvent under reduced pressure to obtain the crude product, and then separate and purify the target product with column chromatography (petroleum ether and ethyl acetate as eluent, with a volume ratio of 4:1) to obtain the target product. 1 was consistent and was not provided in duplicate in 82% yield.
PUM
Login to View More Abstract
Description
Claims
Application Information
Login to View More