HCID 21532578, compound → HCID 12379022, compound

HRID 1658132Notes

Reaction equation

HRID 1658132 reaction equation
[CH2:1]([N:8]1[C:13]2[N:14]=[C:15]([N:18]3[CH2:23][CH2:22][NH:21][CH2:20][CH2:19]3)[N:16]=[CH:17][C:12]=2[C:11](=[O:24])[C:10]([C:25]([O:27]CC)=[O:26])=[CH:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1>S(=O)(=O)(O)O>[CH2:1]([N:8]1[C:13]2[N:14]=[C:15]([N:18]3[CH2:23][CH2:22][NH:21][CH2:20][CH2:19]3)[N:16]=[CH:17][C:12]=2[C:11](=[O:24])[C:10]([C:25]([OH:27])=[O:26])=[CH:9]1)[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

Participants

3

Reactant 1

HCID 21532578HCID 21532578, compound

Product 1

HCID 12379022HCID 12379022, compoundYield 79%

Reagents, catalysts & solvents 1

HCID 1118Sulfuric AcidSolvent

Conditions

Temperature
90 °C

Procedure

Ethyl 8-benzyl-5,8-dihydro-2-(1-piperazinyl)5-oxopyrido[2,3-d]pyrimidine-6-carboxylate (1.5 g) was dissolved in 20 ml of a 12% aqueous solution of sulfuric acid by heating at 90°C for one hour. The resulting solution was filtered to remove a small amount of the insoluble material and the filtrate was neutralized with 28% aqueous ammonia, to separate a solid which was collected, washed with water, and recrystallized from dimethylformamide. There is obtained 1.1 g of the product, m.p. 250° -253°C.

Workup

  1. filtrationThe resulting solution was filtered
  2. customto remove a small amount of the insoluble material
  3. customto separate a solid which
  4. customwas collected
  5. washwashed with water
  6. customrecrystallized from dimethylformamide

Sources & evidence

ORD record
ord-6e134bb9163e4961b7da9695a9709b46
Source dataset
uspto-grants-1976_06
Patent number
US03962443

Reaction notes

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