反应详情

2.74 mL (35.29 mmol) of methanesulfonic acid chloride was added dropwise at 0° C. to a solution of 10.70 g (29.41 mmol) of 2-{4-[5-(4-chlorophenyl)pyridin-2-ylethynyl]-2-methylphenoxy}ethanol and 4.08 mL (29.41 mmol) of triethylamine in 500 mL of THF and the mixture was then stirred for 2 hours at RT. The reaction mixture was filtered and the filtrate was evaporated down in vacuo. The residue was stirred with diethyl ether and water, and the precipitate was filtered off and dried in vacuo. Yield: 11.00 g (85% of theoretical); C23H20ClNO4S (M=441.928); calc.: molpeak (M+H)+: 442/444 (Cl); found: molpeak (M+H)+: 442/444 (Cl); HPLC-MS: 6.36 minutes (method C).

1. filtrationThe reaction mixture was filtered
2. customthe filtrate was evaporated down in vacuo
3. stirringThe residue was stirred with diethyl ether and water
4. filtrationthe precipitate was filtered off
5. customdried in vacuo
6. custom6.36 minutes (method C)