General procedure for the synthesis of ethyl 4,4,4-trifluoro-2-butynoate from ethyl 4,4,4-trifluoro-2-(triphenylphosphoranylidene)acetoacetate:
1. Preparation of reaction materials: ethyl 4,4,4-trifluoro-2-(triphenylphosphoranylidene)acetoacetate (270 g, 617 mmol) and potassium carbonate (54 g, 490 mmol) were weighed.
2. Reaction conditions: The above mixture was heated gradually from 160 °C to 225 °C over a period of 3 h and the reaction was carried out under reduced pressure (mbar vacuum).
3. Isolation of product: Ethyl 4,4,4-trifluoro-2-butynoate was collected by distillation and recovered in a cold trap. 4. Characterization of product: The product was obtained as a shallow product.
4. Characterization of the product: Ethyl 4,4,4-trifluoro-2-butynoate was obtained as a light yellow oil (85 g, 83% yield), the structure of which was confirmed by ES/MS, m/e 167 (M+1).
