A kind of method for preparing fluorine-containing methyl or aryl alkyl ketone
A technology of aryl alkyl ketone and fluorine-containing methyl group, which is applied in the field of organic synthesis, can solve problems such as unavailable, high cost, and difficult recycling, and achieve the effects of avoiding water removal steps, increasing costs, and simplifying the process
- Summary
- Abstract
- Description
- Claims
- Application Information
AI Technical Summary
Problems solved by technology
Method used
Image
Examples
Embodiment 1
[0072] For the synthesis of ethyl 2-ethyl-4,4,4-trifluoroacetoacetate, add 90 g of ethyl n-butyrate to a 250 ml anhydrous and dry four-neck flask, cool down to 0-5 °C with an ice-salt bath, Add 26.3g of solid sodium ethylate, stir at 0-5°C for 1 hour, add dropwise 50g of ethyl trifluoroacetate, keep the temperature at 0-5°C and continue stirring for 1 hour, then raise the temperature to 60-65°C. Stir at -65°C for 24 hours until TFAE<1%, lower the temperature, and concentrate the excess ethyl n-butyrate under reduced pressure to obtain a brown solid, to which 155g of 3NHCl is added dropwise at 20°C until pH≤2. Extracted twice with 100mL 1,2-dichloroethane, concentrated to obtain a brown oily crude product, the crude product was rectified to obtain 49.8g transparent liquid, yield 66.7%, purity: 94.2% (GC).
[0073] For the synthesis of 1,1,1-trifluoro-2-pentanone, 36g (94.2%) of ethyl 2-ethyl-4,4,4-trifluoroacetoacetate was successively added to a 100ml four-neck flask, 14.5 g5...
Embodiment 2
[0076] Synthesis of ethyl 4,4,4-trifluoroacetoacetate, add 69.0g ethyl acetate to a 250ml anhydrous dry four-neck flask, cool down to 0-5°C with an ice-salt bath, add 26.3g solid sodium ethoxide , Stir at 0-5°C for 1 hour, add 50g of ethyl trifluoroacetate dropwise, keep the temperature at 0-5°C and continue stirring for 1 hour, raise the temperature to 60-65°C, and stir at 60-65°C After 24 hours until TFAE<1%, the temperature was lowered, and the excess ethyl acetate was concentrated under reduced pressure to obtain a brown solid, to which 155g of 3NHCl was added dropwise at 20°C until the pH was ≤2. Extracted twice with 100mL 1,2-dichloroethane, concentrated to obtain a brown oily crude product, the crude product was rectified to obtain 45.8g transparent liquid, yield 70.7%, purity: 96.8% (GC).
[0077] Synthesis of 1,1,1-trifluoro-2-propanone, add 36g (94.2%) ethyl 4,4,4-trifluoroacetoacetate, 14.5g 50% sulfuric acid, 36g to a 100ml four-necked flask Acetic acid, set up a ...
Embodiment 3
[0079] Synthesis of ethyl 2-methyl-4,4-difluoroacetoacetate, add 90.5g ethyl propionate to a 250ml anhydrous dry four-neck flask, cool down to 0-5°C with an ice-salt bath, add 30.1 g solid sodium ethoxide, stirred at 0-5°C for 1 hour, added dropwise 50g of ethyl difluoroacetate, kept stirring at 0-5°C for 1 hour after dropping, raised the temperature to 60-65°C, At ℃, stir for 24 hours until DFAE<1%, lower the temperature, and concentrate the excess ethyl propionate under reduced pressure to obtain a brown solid, to which 155g of 3N HCl is added dropwise at 20℃ until the pH≤2. Extracted twice with 100mL 1,2-dichloroethane, concentrated to obtain brown oily crude product, the crude product was rectified to obtain 58.2g transparent liquid, yield 80.0%, purity: 97.3% (GC).
[0080] Synthesis of 1,1-difluoro-2-butanone, add 36g (97.3%) ethyl 2-methyl-4,4-difluoroacetoacetate and 14.5g 50% sulfuric acid to a 100ml four-neck flask , 36g of propionic acid, set up a distillation devi...
PUM
Login to View More Abstract
Description
Claims
Application Information
Login to View More