Ethyl chloroformate → HCID 20326531, compound

HRID 372710Notes

Reaction equation

HRID 372710 reaction equation
[C:1]1([C:7]2[N:12]=[N:11][C:10]([N:13]([CH3:15])[NH2:14])=[CH:9][CH:8]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.C(N(CC)C(C)C)(C)C.Cl[C:26]([O:28][CH2:29][CH3:30])=[O:27]>>[C:1]1([C:7]2[N:12]=[N:11][C:10]([N:13]([CH3:15])[NH:14][C:26]([O:28][CH2:29][CH3:30])=[O:27])=[CH:9][CH:8]=2)[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1

Participants

4

Reactant 3

HCID 10928Ethyl chloroformateHCID 81531DiisopropylethylamineHCID 14273121HCID 14273121, compound

Product 1

HCID 20326531HCID 20326531, compound

Procedure

A solution of 4.4 g. of 6-phenyl-3-(1-methylhydrazino)pyridazine, 3.4 g. of N,N-diisopropylethylamine and 50 ml. of dixane is prepared. To the solution is added 2.6 g. of ethyl chloroformate and the mixture is stirred for 2 hours. The solvent is removed under vacuum and to the residue is added ethanol and water. Filtration gives the product which is recrystallized from ethanol to give crystals, m.p. 129°-130° C.

Workup

  1. customof dixane is prepared
  2. additionTo the solution is added 2.6 g
  3. customThe solvent is removed under vacuum and to the residue
  4. additionis added ethanol and water
  5. filtrationFiltration
  6. customgives the product which
  7. customis recrystallized from ethanol
  8. customto give crystals, m.p. 129°-130° C.

Sources & evidence

ORD record
ord-263886487bea4883a793a9626d8de7a9
Source dataset
uspto-grants-1978_05
Patent number
US04092311

Reaction notes

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