反应详情

温度

70 °C

Under nitrogen replacement, 247 g of 2,3,4-trifluorobromobenzene was dissolved in 740 ml of DMF, into which 247 mL of triethylamine, 3.7 g of tetrakistriphenylphosphine palladium (0), and 4.4 g of copper iodide (I) were added, and heated to 70° C. To this, 108 g of 3-methyl-1-butyne-3-ol was added dropwise for 1 hour, and the mixutre was then stirred for 2 hours at room temperature, for 1 hour at 50° C., for 30 minutes at 60° C., and for 2 hours at 80° C. Then, 500 mL of water was added and cooled to room temperature, to which 200 mL of concentrated hydrochloric acid was added. After this was extracted twice using ethyl acetate, the extract and the organic layer were mixed together, washed using water and a saturated saline solution in that order, and dried using anhydrous magnesium sulfate. After the solvent was evaporated under a reduced pressure, the residue was purified by distillation under a reduced pressure (78 to 84° C./0.65 to 0.70 mmHg) to obtain 229 g of 1-(3-methyl-3-hydroxy-1-butynyl)-2,3,4-trifluorobenzene as a yellow solid.

1. additionwere added
2. waitfor 2 hours at 80° C
3. additionwas added
4. extractionAfter this was extracted twice using ethyl acetate
5. extractionthe extract
6. additionthe organic layer were mixed together
7. washwashed
8. customa saturated saline solution in that order, and dried
9. customAfter the solvent was evaporated under a reduced pressure
10. distillationthe residue was purified by distillation under a reduced pressure (78 to 84° C./0.65 to 0.70 mmHg)