反应详情

温度

-78 °C

To a solution of DMSO (2.07 mmol, 162 mg) in DCM (1.6 mL) at −78° C. was added a solution of oxalyl chloride (1.04 mmol, 131 mg) in DCM (0.2 mL). The mixture was stirred at −78° C. for 15 minutes. Then a solution of (S)—N1-(2-hydroxyethyl)-N1-methyl-N3-(4-(piperidin-1-yl)-2-(4-((1,2,3,4-tetrahydronaphthalen-1-yl)carbamoyl)pyridin-2-yl)phenyl)isophthalamide Example 115 (0.69 mmol, 435 mg) in DCM (0.5 mL) was added. The mixture was stirred at −78° C. for 3 h. Triethylamine (0.5 mL) was added. The mixture was slowly warmed to room temperature. The mixture was diluted with aqueous 10% citric acid and extracted with DCM (3×). The combined organic layers was washed with water (1×), dried, concentrated to give a yellow solid which was used without purification.

1. stirringThe mixture was stirred at −78° C. for 3 h
2. temperatureThe mixture was slowly warmed to room temperature
3. extractionextracted with DCM (3×)
4. washThe combined organic layers was washed with water (1×)
5. customdried
6. concentrationconcentrated
7. customto give a yellow solid which
8. customwas used without purification