Water → HCID 136359197, compound

HRID 1155541Notes

Reaction equation

HRID 1155541 reaction equation
Cl.[NH2:2][OH:3].O.[OH-].[Na+].[CH2:7]([NH:9][C:10]1[CH:15]=[C:14]([C:16](=O)[CH3:17])[CH:13]=[CH:12][N:11]=1)[CH3:8]>CO>[CH2:7]([NH:9][C:10]1[CH:15]=[C:14]([C:16](=[N:2][OH:3])[CH3:17])[CH:13]=[CH:12][N:11]=1)[CH3:8]

Participants

6

Reactant 4

HCID 962WaterHCID 14798Sodium HydroxideHCID 443297Hydroxyamine hydrochlorideHCID 131452661-(2-Ethylamino-4-pyridyl)-1-ethanone

Product 1

HCID 136359197HCID 136359197, compoundYield 87%

Reagents, catalysts & solvents 1

HCID 887MethanolSolvent

Procedure

To a mixture of 7 g. (0.1 mole) of hydroxylamine hydrochloride in 40 ml. of water and 50 ml. of 2 N sodium hydroxide was added 11.5 g. (70 mmoles) of 1-(2-ethylamino-4-pyridyl)-1-ethanone, and the resulting mixture heated to boiling. Methanol was carefully added until the mixture became homogeneous. Heating was continued until the mixture became cloudy. The mixture was cooled and the resulting precipitate filtered, washed with water and dried. Recrystallization from toluene gave 10.9 g. (87%) of the desired product, m.p. 155°-156° C.

Workup

  1. additionTo a mixture of 7 g
  2. temperatureHeating
  3. temperatureThe mixture was cooled
  4. filtrationthe resulting precipitate filtered
  5. washwashed with water
  6. customdried
  7. customRecrystallization from toluene
  8. customgave 10.9 g

Sources & evidence

ORD record
ord-326e57327d40407a9207cc1b20120c85
Source dataset
uspto-grants-1981_11
Patent number
US04302464

Reaction notes

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