1-Bromo-3-methylbutane → HCID 21394525, compound

HRID 1974252Notes

Reaction equation

HRID 1974252 reaction equation
[CH2:1]([N:3]1[C:7]2[N:8]=[CH:9][C:10]3[C:15](=[O:16])[N:14]4[N:17]=[CH:18][CH:19]=[C:13]4[NH:12][C:11]=3[C:6]=2[CH:5]=[N:4]1)[CH3:2].[Na].Br[CH2:22][CH2:23][CH:24]([CH3:26])[CH3:25]>COCCOCCOC>[CH2:1]([N:3]1[C:7]2[N:8]=[CH:9][C:10]3[C:15](=[O:16])[N:14]4[N:17]=[CH:18][CH:19]=[C:13]4[N:12]([CH2:22][CH2:23][CH:24]([CH3:26])[CH3:25])[C:11]=3[C:6]=2[CH:5]=[N:4]1)[CH3:2]

Participants

5

Reactant 3

HCID 78911-Bromo-3-methylbutaneHCID 5360545SodiumHCID 178462996HCID 178462996, compound

Product 1

HCID 21394525HCID 21394525, compound

Reagents, catalysts & solvents 1

HCID 8150DiglymeSolvent

Procedure

7.6 g. of 3-ethyl-3,11-dihydro-6H-pyrazolo[1,5-a]-pyrazolo[4',3':5,6]pyrido[4,3-d]pyrimidin-6-one (0.03 mol.) are refluxed with stirring in 100 ml. of diethyleneglycol dimethylether together with 1.4 g. of sodium (0.06 mol.). After this time, 11.5 g. of 1-bromo-3-methylbutane (0.075 mol) are added and the mixture is refluxed for 16 hours. The solvent is distilled off and the residue is crystallized with methanol, filtered and washed with water to obtain 3-ethyl-3,11-dihydro-11-(3-methylbutyl)-6H-pyrazolo[1,5-a]-pyrazolo[4',3':5,6]pyrido[4,3-d]pyrimidin-6-one, yield 4.1 g. (42%); m.p. 167°-168° (isopropanol).

Workup

  1. temperaturethe mixture is refluxed for 16 hours
  2. distillationThe solvent is distilled off
  3. customthe residue is crystallized with methanol
  4. filtrationfiltered
  5. washwashed with water

Sources & evidence

ORD record
ord-3ad39b5876bc4eedb724fa213b8eae3f
Source dataset
uspto-grants-1976_12
Patent number
US04000277

Reaction notes

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