HCID 13385678, compound → HCID 20227410, compound

HRID 2412915Notes

Reaction equation

HRID 2412915 reaction equation
Cl[C:2]1[C:11]([NH:12][NH2:13])=[N:10][C:9]2[C:4](=[CH:5][C:6]([Cl:15])=[C:7]([Cl:14])[CH:8]=2)[N:3]=1>C(OCC)(OCC)(OCC)CC>[Cl:14][C:7]1([CH2:6][CH3:5])[N:10]2[C:9]3[C:4]([N:3]=[CH:2][C:11]2=[N:12][NH:13]1)=[CH:5][C:6]([Cl:15])=[C:7]([Cl:14])[CH:8]=3

Participants

3

Reactant 1

HCID 13385678HCID 13385678, compound

Product 1

HCID 20227410HCID 20227410, compoundYield 54%

Reagents, catalysts & solvents 1

HCID 66995Ethyl orthopropionateSolvent

Procedure

2,6,7-Trichloro-3-hydrazinoquinoxaline (4.9 g., 0.018 mole) in triethyl orthopropionate (50 ml.) was heated at 100° C. for 2 hours. The precipitate which formed was collected by means of filtration at room temperature and washed with cyclohexane. Recrystallization from chloroform/cyclohexane two times then afforded 2.9 g. (54% yield) of pure 1,7,8-trichloro-1-ethyl-[1,2,4]triazolo[4,3-a]quinoxaline as a pink solid (m.p. 198°-201° C.). Mass spectrum: m/e, 300 (P); m/e, 302 (P+2); m/e, 304 (P+4); m/e, 306 (P+6).

Workup

  1. customThe precipitate which formed
  2. filtrationwas collected by means of filtration at room temperature
  3. washwashed with cyclohexane
  4. customRecrystallization from chloroform/cyclohexane two times
  5. customthen afforded 2.9 g

Sources & evidence

ORD record
ord-a4b28c48c6d2473e8dd628c0b32817ef
Source dataset
uspto-grants-1985_01
Patent number
US04495187

Reaction notes

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