Sodium Methoxide → HCID 178527384, compound

To a solution of 7 g (0.019 mol) 3-(bromodifluoromethylsulfonyl)-1-(N,N-diethylcarbamoyl)-1,2,4-triazole, prepared as in Example 1, in 50 ml methanol at room temperature was added 6.7 ml (0.029 mol) of a 25% w/v solution of sodium methoxide in methanol and the mixture was stirred for 2 h. The reaction mixture was then evaporated and the residue was triturated with ether. The resulting solid was collected by filtration, washed with ether and air-dried. A solution of the above solid in 50 ml water was acidified with concentrated hydrochloric acid and the mixture was extracted with ethyl acetate. The resulting organic layer was washed with saturated sodium chloride solution, dried over MgSO4 and evaporated to give 3.08 g (61% yield) of the desired 3-(bromodifluoromethylsulfonyl)-1,2,4-triazole as a white solid with a melting point of 176-177° C.

1. customThe reaction mixture was then evaporated
2. customthe residue was triturated with ether
3. filtrationThe resulting solid was collected by filtration
4. washwashed with ether
5. customair-dried
6. extractionthe mixture was extracted with ethyl acetate
7. washThe resulting organic layer was washed with saturated sodium chloride solution
8. dry with materialdried over MgSO4
9. customevaporated

ORD record

ord-2a3c01b2d8084e45bfdc3dfe07098ee6

Source dataset

uspto-grants-2002_10

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US06461997B1