反应详情

温度

100 °C

A mixture of 5-(4-bromophenyl)-2-((S)-1-(4fluorophenyl)ethylamino)-5-methylthiazol-4(5H)-one (0.79 g, 1.9 mmol), triphenylphosphine (Aldrich, 0.15 g, 0.58 mmol), palladium acetate (Aldrich, 0.11 g, 0.48 mmol), potassium acetate (Aldrich, 0.24 g, 2.4 mmol), in MeOH (3 mL) and DMF (3 mL) was pressurized with carbon monoxide, purged twice with CO and then heated to 100° C. overnight at 40-50 psi of CO. After the reaction mixture was cooled to ambient temp., then contents were filtered through Celite. The Celite pad was washed with CH2Cl2, and the organic phase was dried over Na2SO4, concentrated in vacuo. The crude material was purified using silica gel chromatography. MS: 387 (M+1).

1. custompurged twice with CO
2. temperatureAfter the reaction mixture was cooled to ambient temp.
3. filtrationcontents were filtered through Celite
4. washThe Celite pad was washed with CH2Cl2
5. dry with materialthe organic phase was dried over Na2SO4
6. concentrationconcentrated in vacuo
7. customThe crude material was purified