Dimethylformamide → HCID 136395950, compound

HRID 2294176Notes

Reaction equation

HRID 2294176 reaction equation
[CH3:1][C:2]1[C:11]([CH3:12])=[CH:10][CH:9]=[C:8]2[C:3]=1[C:4]([N:14]([NH2:20])C(OCC)=O)=[N:5][C:6]([OH:13])=[N:7]2.CN(C)[CH:23]=[O:24]>>[CH3:12][C:11]1[CH:10]=[CH:9][C:8]2[NH:7][C:6](=[O:13])[N:5]3[C:23](=[O:24])[NH:20][N:14]=[C:4]3[C:3]=2[C:2]=1[CH3:1]

Participants

3

Reactant 2

HCID 6228DimethylformamideHCID 178473567HCID 178473567, compound

Product 1

HCID 136395950HCID 136395950, compound

Procedure

0.67 g (0.0020 mol) of ethyl 5,6-dimethyl-2-hydroxy-quinazolin-4-yl-carbazate in 38 ml of dimethylformamide was boiled under reflux for 2 hrs. The reaction mixture was cooled to room temperature and then poured on to ice-water. The precipitate was filtered off and dried in a vacuum. There were obtained white crystals which were recrystallized from methanol/dimethylformamide. Yield: 0.41 g (74%) of 9,10-dimethyl-2,3,5,6-tetrahydro-1,2,4-triazolo[4,3-c]quinazoline-3,5-dione as yellowish crystals; m.p. >350° C.

Workup

  1. temperatureunder reflux for 2 hrs
  2. filtrationThe precipitate was filtered off
  3. customdried in a vacuum
  4. customThere were obtained white crystals which
  5. customwere recrystallized from methanol/dimethylformamide

Sources & evidence

ORD record
ord-b484cdd8454141a18ffd077a2e52e5ef
Source dataset
uspto-grants-1997_11
Patent number
US05688803

Reaction notes

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