Hydrazine → HCID 13914727, compound

HRID 652587Notes

Reaction equation

HRID 652587 reaction equation
[NH2:1][C:2]1[C:11]2[C:6](=[C:7]([Cl:16])[CH:8]=[C:9]([O:14][CH3:15])[C:10]=2[O:12][CH3:13])[N:5]=[C:4](Cl)[N:3]=1.[NH2:18][NH2:19]>CO>[NH2:1][C:2]1[C:11]2[C:6](=[C:7]([Cl:16])[CH:8]=[C:9]([O:14][CH3:15])[C:10]=2[O:12][CH3:13])[N:5]=[C:4]([NH:18][NH2:19])[N:3]=1

Participants

4

Reactant 2

HCID 9321HydrazineHCID 13914720HCID 13914720, compound

Product 1

HCID 13914727HCID 13914727, compoundYield 76.9%

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

A mixture of 4-amino-2,8-dichloro-5,6-dimethoxyquinazoline (1.5 g, 0.0054 moles), anhydrous hydrazine (5 ml, 0.16 moles) and methanol (100 ml) was heated at reflux for 8 hours and stirred at room temperature for 16 hours. The mixture was cooled to 0° C. and the precipitate which formed was collected by filtration. Recrystallization of the solid from methanol followed by drying under vacuum at 55° C. afforded the product (1.12 g), mp 168°-169° C.

Workup

  1. temperaturewas heated
  2. temperatureat reflux for 8 hours
  3. temperatureThe mixture was cooled to 0° C.
  4. customthe precipitate which formed
  5. filtrationwas collected by filtration
  6. customRecrystallization of the solid from methanol
  7. customby drying under vacuum at 55° C.

Sources & evidence

ORD record
ord-e2ea3480e1644e79ba49c3ec285d57d4
Source dataset
uspto-grants-1987_06
Patent number
US04672116

Reaction notes

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