Dimethylformamide → HCID 136395949, compound

HRID 2294174Notes

Reaction equation

HRID 2294174 reaction equation
[OH:1][C:2]1[N:11]=[C:10]([N:12]([NH2:18])C(OCC)=O)[C:9]2[C:4](=[C:5]([CH3:20])[C:6]([CH3:19])=[CH:7][CH:8]=2)[N:3]=1.CN(C)[CH:23]=[O:24]>>[CH3:20][C:5]1[C:4]2[NH:3][C:2](=[O:1])[N:11]3[C:23](=[O:24])[NH:18][N:12]=[C:10]3[C:9]=2[CH:8]=[CH:7][C:6]=1[CH3:19]

Participants

3

Reactant 2

HCID 6228DimethylformamideHCID 178473569HCID 178473569, compound

Product 1

HCID 136395949HCID 136395949, compound

Procedure

3.88 g (0.012 mol) of ethyl 2-hydroxy-7,8-dimethylquinazoline-4-yl-carbazate in 220 ml of dimethylformamide were 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 dimethylformamide. Yield: 1.62 g (50%) of 7,8-dimethyl-2,3,5,6-tetrahydro-1,2,4-triazolo[4,3-c]quinazoline-3,5-dione as yellowish crystals; m.p. 380°-382° 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 dimethylformamide

Sources & evidence

ORD record
ord-5c448fd956dc457ca2da81a5d9932cfa
Source dataset
uspto-grants-1997_11
Patent number
US05688803

Reaction notes

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