Pyridine → HCID 57562419, compound

Temperature

0 °C

112 μl (1.2 eq; 0.667 mmol) of trifluoromethanesulfonic anhydride and 337 μl (17.5 eq; 49.557 mmol) of pyridine, under an argon atmosphere, are added dropwise to a solution of 98 mg (1 eq; 0.556 mmol) of 1-(5-hydroxyindazol-1-yl)ethanone in 10 ml of dichloromethane on amylene, pre-cooled to 0° C. The medium is stirred and kept at 0° C. overnight under an argon atmosphere. 112 μl of trifluoromethanesulfonic anhydride and 337 μl of pyridine are added to the medium, which is stirred for 2 hours at 0° C. 112 μl of trifluoromethanesulfonic anhydride and 337 μl of pyridine are then added, and the medium is then stirred for 3 hours at 0° C. The reaction mixture is washed with 10 ml of water. The aqueous phase is treated with 2 times 10 ml of dichloromethane. The organic phase is dried over magnesium sulfate and then filtered and the solvent is evaporated off under reduced pressure in a rotary evaporator to obtain 168.9 mg of trifluoromethanesulfonic acid 1-acetyl-1H-indazol-5-yl ester are obtained.

1. stirringis stirred for 2 hours at 0° C
2. stirringthe medium is then stirred for 3 hours at 0° C
3. washThe reaction mixture is washed with 10 ml of water
4. additionThe aqueous phase is treated with 2 times 10 ml of dichloromethane
5. dry with materialThe organic phase is dried over magnesium sulfate
6. filtrationfiltered
7. customthe solvent is evaporated off under reduced pressure in a rotary evaporator

ORD record

ord-a9501db757b445ff9b62a13201752546

Source dataset

uspto-grants-2009_02

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US07491710B2