Hydrochloric Acid → 3-Butyn-2-ol, 1,1,1-trifluoro-4-phenyl-

Temperature

-78 °C

In a solution of phenylacetylene (4.08 g, 40 mmol) in dry ether (30 ml), n-butyllithium (27 ml, 1.5 M in hexane) was slowly added at -78° C. Trifluoroacetaldehyde (3.7 g, 38 mmol) was introduced in the above mixture under bubbling and the mixture was then agitated 2 hours at -78° C. After the temperature of reaction mixture was elevated to room temperature, the whole solution was poured into aqueous 2% HCl solution. Extraction was made for the oily layer using diethyl ether. The extracts were dried on magnesium sulfate and solvent was removed. Distillation gave 1,1,1-trifluoro-4-phenyl-3-butyne-2-ol (b.p.: 82° C./1.8 mmHg) at a yield of 74%. The above product gave the following analytical data:

1. customunder bubbling
2. customAfter the temperature of reaction mixture
3. customwas elevated to room temperature
4. extractionExtraction
5. customThe extracts were dried on magnesium sulfate and solvent
6. customwas removed
7. distillationDistillation

ORD record

ord-926e0539dbff4c57879efbbd2f8fc611

Source dataset

uspto-grants-1985_07

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US04532020