Methyl Isocyanate → HCID 12904737, compound

HRID 1679902Notes

Reaction equation

HRID 1679902 reaction equation
[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([Cl:8])[C:3]=1[C:9]1[C:19]([NH2:20])=[N:18][C:12]2[N:13]=[C:14]([CH3:17])[N:15]=[CH:16][C:11]=2[CH:10]=1.[CH3:21][N:22]=[C:23]=[O:24]>CCOCC>[Cl:8][C:4]1[CH:5]=[CH:6][CH:7]=[C:2]([Cl:1])[C:3]=1[C:9]1[C:19]([NH:20][C:23]([NH:22][CH3:21])=[O:24])=[N:18][C:12]2[N:13]=[C:14]([CH3:17])[N:15]=[CH:16][C:11]=2[CH:10]=1

Participants

4

Reactant 2

HCID 12228Methyl IsocyanateHCID 12904727HCID 12904727, compound

Product 1

HCID 12904737HCID 12904737, compound

Reagents, catalysts & solvents 1

HCID 3283Diethyl EtherSolvent

Procedure

A slurry of 3.0 g of 6-(2,6-dichlorophenyl)-2-methylpyrido[2,3-d]-pyrimidin-7-amine in 20 ml of methyl isocyanate is heated at reflux for 3 hours to obtain a yellow solution. This is stirred overnight at room temperature and diluted with 20 ml of ether. The solvent and excess isocyanate are evaporated and the solid residue of crude product is purified by recrystallization from ethyl acetate to give N-[6-(2,6-dichlorophenyl)-2-methylpyrido[2,3-d]-pyrimidin-7-yl]-N'-methylurea, mp 168°-171° C. (dec.).

Workup

  1. temperatureat reflux for 3 hours
  2. customto obtain a yellow solution
  3. customThe solvent and excess isocyanate are evaporated
  4. customthe solid residue of crude product is purified by recrystallization from ethyl acetate

Sources & evidence

ORD record
ord-15a6acf1ae0f4c83bb0f5d1f3a155883
Source dataset
uspto-grants-1981_06
Patent number
US04271164

Reaction notes

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