Ethanol → HCID 178481355, compound

HRID 476916Notes

Reaction equation

HRID 476916 reaction equation
[C:1]([C:3]1[C:4](=[O:17])[N:5]([CH3:16])[C:6](=[O:15])[N:7]([CH3:14])[C:8]=1[N:9]=[CH:10][N:11](C)C)#[N:2].Cl.ON.C(N(CC)CC)C.C([OH:30])C>O>[NH2:2][C:1]1[N+:11]([O-:30])=[CH:10][N:9]=[C:8]2[N:7]([CH3:14])[C:6](=[O:15])[N:5]([CH3:16])[C:4](=[O:17])[C:3]=12

Participants

6

Reactant 4

HCID 702EthanolHCID 8471TriethylamineHCID 443297Hydroxyamine hydrochlorideHCID 53948848HCID 53948848, compound

Product 1

HCID 178481355HCID 178481355, compoundYield 85%

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Procedure

0.235 g (1 mmol) of the compound 15, 0.138 g (2 mmol) of hydroxyamine hydrochloride and 0.243 g (2.4 mmol) of triethylamine were added to 3 ml of ethanol, and then the reaction mixture was refluxed for 3 hours. After cooling, 5 ml of water was added thereto, and the crystalline precipitate was filtered off and recrystallized from ethanol to give 0.223 g of 5-amino-1,3-dimethylpyrimido[4,5-d]pyrimidine-2,4-dione-6-oxide in a 85% yield.

Workup

  1. temperaturethe reaction mixture was refluxed for 3 hours
  2. temperatureAfter cooling
  3. filtrationthe crystalline precipitate was filtered off
  4. customrecrystallized from ethanol

Sources & evidence

ORD record
ord-8bf3cedc24824ce59fa773bcd865448a
Source dataset
uspto-grants-1989_12
Patent number
US04886807

Reaction notes

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