Sodium ethoxide → HCID 58045754, compound

HRID 657886Notes

Reaction equation

HRID 657886 reaction equation
Cl[C:2]1[C:11]2[CH2:10][CH2:9][CH2:8][CH2:7][C:6]=2[C:5]2=[N:12][N:13]=[C:14]([NH2:15])[N:4]2[N:3]=1.[O-:16][CH2:17][CH3:18].[Na+]>C(O)C>[CH2:17]([O:16][C:2]1[C:11]2[CH2:10][CH2:9][CH2:8][CH2:7][C:6]=2[C:5]2=[N:12][N:13]=[C:14]([NH2:15])[N:4]2[N:3]=1)[CH3:18]

Participants

4

Reactant 2

HCID 2723922Sodium ethoxideHCID 15107886HCID 15107886, compound

Product 1

HCID 58045754HCID 58045754, compoundYield 47.1%

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

6-Chloro-7,8,9,10-tetrahydro-[1,2,4]triazolo[3,4-a]phthalazin-3-ylamine (W2.018, 1.0 g) was dissolved in ethanol (50 ml) while stirring and under argon. Thereafter, the reaction mixture was admixed with sodium ethoxide (1.34 g) and stirred at 60° C. for 1 h. After the solvent had been drawn off, the residue was purified using a 40 g silica gel cartridge (0-20% dichloromethane-ethanol gradient in 40 min). The clean product fractions were combined and dried. 491 mg of the title compound were obtained.

Workup

  1. stirringstirred at 60° C. for 1 h
  2. customthe residue was purified
  3. customa 40 g silica gel cartridge (0-20% dichloromethane-ethanol gradient in 40 min)
  4. customdried

Sources & evidence

ORD record
ord-4c7610a331dc45e8930e4f455af7277b
Source dataset
uspto-grants-2011_12
Patent number
US08076336B2

Reaction notes

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