N-methylhydroxylamine hydrochloride → HCID 20532869, compound

HRID 1758889Notes

Reaction equation

HRID 1758889 reaction equation
[CH3:1][C:2]1[CH:13]=[C:12]([N+:14]([O-:16])=[O:15])[C:5]([NH:6][CH:7]([CH3:11])[C:8](Cl)=[O:9])=[C:4]([N+:17]([O-:19])=[O:18])[CH:3]=1.Cl.[CH3:21][NH:22][OH:23].C([O-])(=O)C.[Na+]>C(Cl)Cl.O>[CH3:21][N:22]([C:8](=[O:9])[CH:7]([NH:6][C:5]1[C:12]([N+:14]([O-:16])=[O:15])=[CH:13][C:2]([CH3:1])=[CH:3][C:4]=1[N+:17]([O-:19])=[O:18])[CH3:11])[OH:23]

Participants

6

Reactant 3

HCID 77906N-methylhydroxylamine hydrochlorideHCID 517045Sodium AcetateHCID 20532868HCID 20532868, compound

Product 1

HCID 20532869HCID 20532869, compound

Reagents, catalysts & solvents 2

HCID 962WaterSolventHCID 6344DichloromethaneSolvent

Procedure

A solution of 2.0 g of 2-(4-methyl-2,6-dinitroanilino)propionyl chloride, prepared as in Example 1, in 50 ml of methylene chloride was added dropwise to a stirred solution of 2.0 g of N-methylhydroxylamine hydrochloride and 6.0 g of sodium acetate in 50 ml of water at 0°-5° C. The mixture was stirred for 2 hours, after which the organic layer was spearated, dried and evaporated to dryness. The yellow residue was recrystallised from benzene to give 3, m.p.: 171°-172° C.

Workup

  1. customdried
  2. customevaporated to dryness
  3. customThe yellow residue was recrystallised from benzene
  4. customto give 3, m.p.: 171°-172° C.

Sources & evidence

ORD record
ord-38a7d8d521414e0f8e8378932c5d0860
Source dataset
uspto-grants-1982_07
Patent number
US04338121

Reaction notes

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