Water → HCID 54276338, compound
Reaction equation
[H-].[Na+].N1C=[CH:6][N:5]=[N:4]1.[CH3:8][C:9]([CH3:23])([C:11](=[O:22])[CH:12](Br)[CH:13](Br)[C:14](=[O:19])[C:15]([CH3:18])([CH3:17])[CH3:16])[CH3:10].O.[CH3:25][N:26](C)C=O>>[N:5]1([C:12](=[CH:13][C:14](=[O:19])[C:15]([CH3:18])([CH3:17])[CH3:16])[C:11](=[O:22])[C:9]([CH3:23])([CH3:10])[CH3:8])[CH:6]=[N:26][CH:25]=[N:4]1Participants
6
Procedure
Sodium hydride (100, %%, 0.06 mol) was added to a suspension of triazole (0.06 mol) in dimethyl formamide (100 ml) and the solution stirred at 20° until effervescence ceased. 2,2,7,7-Tetramethyl-4,5,dibromo-octan-3,6-dione (0.03 mol) was added portionwise at 20° to the stirred solution. After refluxing for 2 hours, the solution was cooled and poured into water to give a crystalline solid. Recrystallization from petroleum ether (60°-80°) gave the title compound as a white crystalline solid, m.p. 107°-8°.
Workup
- temperatureAfter refluxing for 2 hours
- temperaturethe solution was cooled
- customto give a crystalline solid
- customRecrystallization from petroleum ether (60°-80°)
Sources & evidence
- ORD record
- ord-2e7f595be306435b98f400658b09d337
- Source dataset
- uspto-grants-1981_01
- Patent number
- US04246020
Reaction notes
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