HCID 13424594, compound → HCID 22768931, compound

HRID 1764634Notes

Reaction equation

HRID 1764634 reaction equation
Cl[C:2]1[N:7]=[N:6][C:5]([C:8]2[CH:15]=[CH:14][C:11]([C:12]#[N:13])=[CH:10][CH:9]=2)=[C:4]([CH3:16])[CH:3]=1>C(O)CCC>[CH2:4]([C:5]1[N:7]2[N:6]=[C:5]([C:8]3[CH:15]=[CH:14][C:11]([C:12]#[N:13])=[CH:10][CH:9]=3)[C:4]([CH3:16])=[CH:3][C:2]2=[N:7][N:6]=1)[CH3:3]

Participants

3

Reactant 1

HCID 13424594HCID 13424594, compound

Product 1

HCID 22768931HCID 22768931, compound

Reagents, catalysts & solvents 1

HCID 2631-ButanolSolvent

Procedure

A 30.8 g. portion of the above compound is dissolved in one liter of butyl alcohol (dried over 3-A molecular sieves), then 40.0 g. of p-(6-chloro-4-methyl-3-pyridazinyl)-benzonitrile (prepared as in Example 1) is added and the reaction mixture is allowed to heat at reflux for 18 hours. The reaction mixture is concentrated free of solvent and the concentrate is triturated with petroleum ether, then is filtered. The filter cake is vacuum dried to afford a yellow solid which is then recrystallized from methyl alcohol to give the product of the example, m.p. 192°-195° C.

Workup

  1. temperatureto heat
  2. temperatureat reflux for 18 hours
  3. concentrationThe reaction mixture is concentrated free of solvent
  4. customthe concentrate is triturated with petroleum ether
  5. filtrationis filtered
  6. customdried
  7. customto afford a yellow solid which
  8. customis then recrystallized from methyl alcohol
  9. customto give the product of the example, m.p. 192°-195° C.

Sources & evidence

ORD record
ord-9c40664d59d244889097caa9836bd302
Source dataset
uspto-grants-1978_09
Patent number
US04117130

Reaction notes

Loading…