Hydroxyamine hydrochloride → HCID 86070635, compound

HRID 910364Notes

Reaction equation

HRID 910364 reaction equation
[CH:1]([C:3]1[CH:18]=[CH:17][C:6]([C:7]([NH:9][CH2:10][C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][N:12]=2)=[O:8])=[C:5]([CH3:19])[CH:4]=1)=O.Cl.[OH:21][NH2:22]>C(O)C.O>[OH:21][N:22]=[CH:1][C:3]1[CH:18]=[CH:17][C:6]([C:7]([NH:9][CH2:10][C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][N:12]=2)=[O:8])=[C:5]([CH3:19])[CH:4]=1

Participants

5

Reactant 2

HCID 443297Hydroxyamine hydrochlorideHCID 86611467HCID 86611467, compound

Product 1

HCID 86070635HCID 86070635, compoundYield 85%

Reagents, catalysts & solvents 2

HCID 702EthanolSolventHCID 962WaterSolvent

Procedure

In a solution of 0.50 g of 4-formyl-2-methyl-N-(2-pyridylmethyl)benzoic acid amide in 10 ml of ethanol and 5 ml of water, 0.18 g of hydroxyamine hydrochloride was added with stirring at room temperature, and stirred at the same temperature for 12 hours. After the completion of the reaction, solid was filtered off, ethanol was distilled off under reduced pressure, and 30 ml of saturated sodium hydrogen carbonate aqueous solution was added in the remaining aqueous solution. The precipitated crystal was filtered off, washed with water and dried to obtain 0.45 g of the aimed product as pale yellow crystal.

Workup

  1. stirringstirred at the same temperature for 12 hours
  2. customAfter the completion of the reaction, solid
  3. filtrationwas filtered off
  4. distillationethanol was distilled off under reduced pressure, and 30 ml of saturated sodium hydrogen carbonate aqueous solution
  5. additionwas added in the remaining aqueous solution
  6. filtrationThe precipitated crystal was filtered off
  7. washwashed with water
  8. customdried

Sources & evidence

ORD record
ord-9288636fd39f4f5eb70136a13a9a6070
Source dataset
uspto-grants-2011_09
Patent number
US08022089B2

Reaction notes

Loading…