Dimethylamine → HCID 135670776, compound

HRID 1936650Notes

Reaction equation

HRID 1936650 reaction equation
CS[C:3]1[N:8]=[C:7]2[N:9]=[C:10]([C:14]3[CH:19]=[CH:18][CH:17]=[CH:16][C:15]=3[O:20][CH2:21][CH2:22][CH3:23])[NH:11][C:12](=[O:13])[C:6]2=[CH:5][N:4]=1.[CH3:24][NH:25][CH3:26]>[OH-].[Na+].Cl>[CH3:24][N:25]([CH3:26])[C:3]1[N:8]=[C:7]2[N:9]=[C:10]([C:14]3[CH:19]=[CH:18][CH:17]=[CH:16][C:15]=3[O:20][CH2:21][CH2:22][CH3:23])[NH:11][C:12](=[O:13])[C:6]2=[CH:5][N:4]=1

Participants

5

Reactant 2

HCID 674DimethylamineHCID 1355223017-Methylthio-4-oxo-2-(2-propoxyphenyl)-3,4-dihydropyrimido[4,5-d]pyrimidine

Product 1

HCID 135670776HCID 135670776, compound

Reagents, catalysts & solvents 2

HCID 313Hydrochloric AcidCatalystHCID 14798Sodium HydroxideSolvent

Procedure

7-Methylthio-4-oxo-2-(2-propoxyphenyl)-3,4-dihydropyrimido[4,5-d]pyrimidine (0.60 g) was treated with a solution of dimethylamine in industrial methylated spirit (33%; 20 ml) in a pressure vessel for 18 hours at 90° C. The cooled reaction mixture was evaporated under reduced pressure to yield a solid which was dissolved in aqueous sodium hydroxide. The filtered aqueous solution was neutralized with a few drops of concentrated hydrochloric acid to yield a pale yellow solid which was recrystallized from 2-propanol to yield the title compound, 0.33 g, m.p. 177.5-178.5° C.

Workup

  1. customThe cooled reaction mixture
  2. customwas evaporated under reduced pressure
  3. customto yield a solid which
  4. customto yield a pale yellow solid which
  5. customwas recrystallized from 2-propanol

Sources & evidence

ORD record
ord-2b07839476344505beac7ea69a0d5c24
Source dataset
uspto-grants-2002_05
Patent number
US06391885B1

Reaction notes

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