2-Methylmorpholine → HCID 12246651, compound

HRID 1973654Notes

Reaction equation

HRID 1973654 reaction equation
Cl[C:2]1[N:7]=[N:6][C:5](Cl)=[C:4]2[CH:9]=[N:10][C:11]([C:13]3[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=3)=[CH:12][C:3]=12.[CH3:19][CH:20]1[O:25][CH2:24][CH2:23][NH:22][CH2:21]1>>[CH3:19][CH:20]1[CH2:21][N:22]([C:2]2[N:7]=[N:6][C:5]([N:22]3[CH2:23][CH2:24][O:25][CH:20]([CH3:19])[CH2:21]3)=[C:4]3[CH:9]=[N:10][C:11]([C:13]4[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=4)=[CH:12][C:3]=23)[CH2:23][CH2:24][O:25]1

Participants

3

Reactant 2

HCID 4106152-MethylmorpholineHCID 12246632HCID 12246632, compound

Product 1

HCID 12246651HCID 12246651, compound

Procedure

2.0 parts by weight of 1,4-dichloro-7-phenylpyrido(3,4-d)pyridazine is added to 20 parts by volume of 2-methylmorpholine, and the resulting mixture is heated at 130° to 140° C for 4 hours. The excess amount of 2-methylmorpholine is removed by evaporation under reduced pressure. Water is added to the residue to obtain crude crystals, which is recrystallized from n-hexane to obtain 1,4-bis(2'-methylmorpholino)-7-phenylpyrido(3,4-d)pyridazine as yellow prisms melting at 75° to 81° C. Elementary analysis for C23H27O2N5

Workup

  1. temperaturethe resulting mixture is heated at 130° to 140° C for 4 hours
  2. customThe excess amount of 2-methylmorpholine is removed by evaporation under reduced pressure
  3. additionWater is added to the residue
  4. customto obtain crude crystals, which
  5. customis recrystallized from n-hexane

Sources & evidence

ORD record
ord-059be1d437894e32ae97c542c41a7c38
Source dataset
uspto-grants-1976_12
Patent number
US03998822

Reaction notes

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