Water → 9-[4-(Cyclohexyloxy)phenyl]-3,4-dihydropyrido[2,1-c][1,2,4]thiadiazine 2,2-dioxide

Temperature

60 °C

A solution of 2-chloroethanesulfonyl chloride (381 mg) in N,N-dimethylacetoamide (2 mL) was added dropwise to a suspension of 3-[4-(cyclohexyloxy)phenyl]pyridin-2-amine (301 mg) in N,N-dimethylacetoamide (2 ml) and additional N,N-dimethylacetoamide (1 mL) was used to complete the addition of above solution. After being stirred at 60° C. for 3 hr, the mixture was cooled to room temperature. Water (10 mL) was added dropwise to the reaction mixture and the whole was stirred at room temperature for 0.5 hr. The precipitate was collected by filtration, washed with water (10 mL) and diisopropyl ether (3 ml), and dried in vacuo at 60° C. to give the title compound (342 mg) as an off-white powder.

1. additionthe addition of above solution
2. temperaturethe mixture was cooled to room temperature
3. stirringthe whole was stirred at room temperature for 0.5 hr
4. filtrationThe precipitate was collected by filtration
5. washwashed with water (10 mL) and diisopropyl ether (3 ml)
6. customdried in vacuo at 60° C.

ORD record

ord-3f9a051ad44142e9aa020a891c47637c

Source dataset

uspto-grants-2014_07

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08778934B2