Water → HCID 12056494、化合物

To a solution of 57 g (0.17 mol) 3-(bromodifluoromethylthio)-1-(N,N-diethylcarbamoyl)-1,2,4-triazole, prepared as above, in 100 ml acetonitrile were sequentially added 100 ml carbon tetrachloride, 200 ml water and 11 1.23 g (0.52 mol) sodium periodate. To the resulting suspension was added 20 mg (ca 5 mol %) ruthenium trichloride hydrate and the suspension was then stirred at room temperature for 24 h. The reaction mixture was then diluted with 500 ml water, extracted with dichloromethane (3×200 ml) and the combined resulting organic layers were sequentially washed with water, saturated sodium bicarbonate solution and brine. The dichloromethane solution was dried over MgSO4 and evaporated. Preparative LC purification of the residue with 40% ethyl acetate-hexane gave 53.31 g (85% yield) of the desired 3-(bromodifluoromethylsulfonyl)-1-(N,N-diethylcarbamoyl)-1,2,4-triazole as a white solid with melting point 74-75° C.

1. extractionextracted with dichloromethane (3×200 ml)
2. customthe combined resulting organic layers
3. washwere sequentially washed with water, saturated sodium bicarbonate solution and brine
4. dry with materialThe dichloromethane solution was dried over MgSO4
5. customevaporated
6. customPreparative LC purification of the residue with 40% ethyl acetate-hexane

ORDレコード

ord-874809369a914d5795732caf3b4488c0

出典データセット

uspto-grants-2002_10

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US06461997B1