Acetic Acid → HCID 135670802, compound

HRID 1107337Notes

Reaction equation

HRID 1107337 reaction equation
CS([C:5]1[N:10]=[C:9]2[N:11]=[C:12]([C:16]3[CH:21]=[CH:20][CH:19]=[CH:18][C:17]=3[O:22][CH2:23][CH2:24][CH3:25])[NH:13][C:14](=[O:15])[C:8]2=[CH:7][N:6]=1)(=O)=O.[C:26](O)(=[O:28])[CH3:27]>[O-]CC.[Na+]>[CH2:26]([O:28][C:5]1[N:10]=[C:9]2[N:11]=[C:12]([C:16]3[CH:21]=[CH:20][CH:19]=[CH:18][C:17]=3[O:22][CH2:23][CH2:24][CH3:25])[NH:13][C:14](=[O:15])[C:8]2=[CH:7][N:6]=1)[CH3:27]

Participants

4

Procedure

A solution of 7-methylsulphonyl-4-oxo-2-(2-propoxyphenyl)-3,4-dihydropyrimido[4,5-d]pyrimidine (0.50 g) in sodium ethoxide solution (from sodium, 0.16 g, and ethanol, 25 ml) was stirred at ambient temperature for 1.5 hours. Cooling and acidification of the reaction mixture with glacial acetic acid (0.42 g) yielded a precipitate which was twice recrystallized from ethanol to yield the title compound, 0.29 g, m.p. 196-197.5° C.

Workup

  1. temperatureCooling
  2. customwas twice recrystallized from ethanol

Sources & evidence

ORD record
ord-8b6bfc33e0fa498a8284f3eb5e173dc3
Source dataset
uspto-grants-2000_05
Patent number
US06060477

Reaction notes

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