Sodium hydride → HCID 178424719, compound

HRID 449797Notes

Reaction equation

HRID 449797 reaction equation
[CH3:1][C:2]1[C:3]([N+:15]([O-:17])=[O:16])=[C:4]([CH:12]=[CH:13][CH:14]=1)[C:5]([NH:7][O:8][CH2:9][CH2:10]Cl)=[NH:6].[H-].[Na+]>CN1CCCC1=O>[CH3:1][C:2]1[C:3]([N+:15]([O-:17])=[O:16])=[C:4]([C:5]2[NH:6][CH2:10][CH2:9][O:8][N:7]=2)[CH:12]=[CH:13][CH:14]=1

Participants

4

Reactant 2

HCID 24758Sodium hydrideHCID 178425258HCID 178425258, compound

Product 1

HCID 178424719HCID 178424719, compound

Reagents, catalysts & solvents 1

HCID 13387N-methyl-2-pyrrolidoneSolvent

Conditions

Temperature
100 °C

Procedure

1.4 g (5.4 mmol) of 3-methyl-N-(2-chloroethoxy)-2-nitrobenzamidine are initially charged in 45 ml of 1-methyl-2-pyrrolidone, and 0.18 g (6 mmol) of sodium hydride (80% pure) is added slowly. The mixture is stirred at 100° C. for 12 h, cooled, poured onto water and extracted with ethyl acetate. After drying over sodium sulphate, the solvent is distilled off under reduced pressure.

Workup

  1. temperaturecooled
  2. additionpoured onto water
  3. extractionextracted with ethyl acetate
  4. dry with materialAfter drying over sodium sulphate
  5. distillationthe solvent is distilled off under reduced pressure

Sources & evidence

ORD record
ord-e4baf6c25454498796e916d5f6fe4800
Source dataset
uspto-grants-2013_07
Patent number
US08486934B2

Reaction notes

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