Sulfuric Acid → HCID 22642151, compound
Reaction equation
[NH:1]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[C:4](=[O:11])[NH:3][C:2]1=[O:12].[S:13](=O)(=[O:16])([OH:15])[OH:14]>>[O:12]=[C:2]1[NH:3][C:4](=[O:11])[C:5]2[C:10](=[CH:9][CH:8]=[C:7]([S:13]([OH:16])(=[O:15])=[O:14])[CH:6]=2)[NH:1]1Participants
3
Procedure
2,4(1H, 3H)-Quinazolinedione (10 g) was added portionwise to a stirred mixture of 65% fuming sulphuric acid (10 ml) and concentrated sulphuric acid (40 ml) at room temperature. After the addition was complete, the mixture was stirred at 55°-60° for 30 minutes, cooled, poured onto ice (100 g) and stood in a refrigerator for 1 hour. The colourless crystals were filtered, washed with a little ice-cold 6 N hydrochloric acid and finally dried in a vacuum oven to give the hydrated title compound, (14.7 g, m.p. >300°).
Workup
- additionAfter the addition
- temperaturecooled
- additionpoured onto ice (100 g)
- waitstood in a refrigerator for 1 hour
- filtrationThe colourless crystals were filtered
- washwashed with a little ice-cold 6 N hydrochloric acid
- customfinally dried in a vacuum oven
Sources & evidence
- ORD record
- ord-99a70e55720748c0b5da0663ef85a33b
- Source dataset
- uspto-grants-1981_05
- Patent number
- US04267325
Reaction notes
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