反应详情

Sodium hydride (60% in mineral oil; 0.042 g, 1.04 mmol) was suspended in DMF (5 mL). After stirring for 10 minutes, 2-methyl-2-propanethiol (0.13 mL, 1.15 mmol) was added, and the mixture was stirred for 30 minutes. (5-{2-[(N-Cyclopropanecarbonyl-N-ethyl-amino)-methyl]-4-fluoro-phenyl}-pyridin-3-yl)-acetic acid ethyl ester (0.20 g, 0.52 mmol) was added, and the reaction was stirred at 90° C. overnight. The mixture was diluted with H2O, and N2 was bubbled through the solution into a bleach trap until all odor was removed. The aqueous layer was washed with EtOAc, and then acidified to pH 4 and extracted with EtOAc. The combined organic layers were concentrated, and the residue was purified by preparative HPLC to give Compound 22.

1. stirringthe mixture was stirred for 30 minutes
2. stirringthe reaction was stirred at 90° C. overnight
3. customwas bubbled through the solution into a bleach trap until all odor
4. customwas removed
5. washThe aqueous layer was washed with EtOAc
6. extractionextracted with EtOAc
7. concentrationThe combined organic layers were concentrated
8. customthe residue was purified by preparative HPLC