Ammonia → HCID 13060457, compound

HRID 2296429Notes

Reaction equation

HRID 2296429 reaction equation
[Cl:1][C:2]1[N:11]=[C:10](Cl)[C:9]2[C:4](=[CH:5][CH:6]=[C:7]([CH2:13][CH3:14])[CH:8]=2)[N:3]=1.[NH3:15].O>CO.C(Cl)(Cl)Cl>[NH2:15][C:10]1[C:9]2[C:4](=[CH:5][CH:6]=[C:7]([CH2:13][CH3:14])[CH:8]=2)[N:3]=[C:2]([Cl:1])[N:11]=1

Participants

6

Reactant 3

HCID 222AmmoniaHCID 962WaterHCID 130605152,4-Dichloro-6-ethylquinazoline

Product 1

HCID 13060457HCID 13060457, compound

Reagents, catalysts & solvents 2

HCID 887MethanolSolventHCID 6212ChloroformSolvent

Procedure

A solution of 2,4-dichloro-6-ethylquinazoline (10.8 g) in methanol and chloroform (70 ml ) was cooled with ice-water. Ammonia was passed through the reaction mixture for 20 minutes and the mixture was allowed to stand for 18 hours at ambient temperature. The resultant mixture was concentrated under reduced pressure to give a residue, to which was added water and heated to 50°-60° C. with stirring. The precipitates was separated by filtration, washed with hot water and recrystallized from dioxane to give crystalline 4-amino-2-chloro-6-ethylquinazoline (8.3 g). Crystals (0.7 g) of the same compound were obtained by treating the mother liquor in substantially the same manner as mentioned above.

Workup

  1. concentrationThe resultant mixture was concentrated under reduced pressure
  2. customto give a residue
  3. temperatureheated to 50°-60° C.
  4. customThe precipitates was separated by filtration
  5. washwashed with hot water
  6. customrecrystallized from dioxane

Sources & evidence

ORD record
ord-a8b52944c4a94e85a1db21e157df3697
Source dataset
uspto-grants-1984_01
Patent number
US04429126

Reaction notes

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