Nitric Acid → HCID 19980149, compound
Reaction equation
[N+:1]([O-:4])(O)=[O:2].S(=O)(=O)(O)O.[CH3:10][N:11]1[C:15](=[O:16])[C:14]([CH2:17][Cl:18])=[C:13]([C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=2)[O:12]1>>[CH3:10][N:11]1[C:15](=[O:16])[C:14]([CH2:17][Cl:18])=[C:13]([C:19]2[CH:24]=[CH:23][C:22]([N+:1]([O-:4])=[O:2])=[CH:21][CH:20]=2)[O:12]1Participants
4
Procedure
After cooling 76 ml of concentrated nitric acid (specific gravity 1.42) to 0° C., 80 ml of concentrated sulfuric acid was gradually added thereto and further 9 g of 2-methyl-4 chloromethyl-5-phenyl-3-isooxazolone was added thereto as crystals thereof while keeping the temperature thereof below 5° C. The resultant mixture was stirred for 30 minutes at 5° C. and poured into 2 liters of ice water followed by stirring for one hour to deposit crystals, which were collected by filtration and dried to provide 9.4 g of the desired product. The yield was 87%.
Workup
- custombelow 5° C
- filtrationwere collected by filtration
- customdried
Sources & evidence
- ORD record
- ord-4376206c4ca1435989cd615c67b41040
- Source dataset
- uspto-grants-1991_12
- Patent number
- US05075208
Reaction notes
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