反应详情

温度

-78 °C

To a of solution of 5-(3,3-dimethyl-but-1-ynyl)-thiophene-2-carboxylic acid (6.5 g, 31.3 mmol, 1.0 equiv) in THF (150 mL) at −78° C. was added n-BuLi (44.9 mL, 1.6 M in heptane, 71.9 mmol, 2.3 equiv) and the resulting solution was stirred at −78° C. for 1 hour. To the solution was then added 1,2-dibromo-1,1,2,2-tetrafluoro-ethane (16.2 g, 62.5 mmol, 2.0 equiv) and the solution was allowed to warm to room temperature over 2 hours. The reaction was quenched by addition of sat. aq. NH4Cl solution and the mixture was extracted with EtOAc. The organic layers were combined, washed with brine, dried over Na2SO4 and concentrated. The crude material was continued to the next step with no further purification.

1. temperatureto warm to room temperature over 2 hours
2. customThe reaction was quenched by addition of sat. aq. NH4Cl solution
3. extractionthe mixture was extracted with EtOAc
4. washwashed with brine
5. dry with materialdried over Na2SO4
6. concentrationconcentrated
7. customThe crude material was continued to the next step with no further purification