Hydroxylamine, sulfate (1:1) → HCID 74057258, compound

HRID 1836111Notes

Reaction equation

HRID 1836111 reaction equation
[CH:1]1([C:6](=O)[CH2:7][N+:8]([O-:10])=[O:9])[CH2:5][CH2:4][CH2:3][CH2:2]1.S(O)(O)(=O)=O.[NH2:17][OH:18]>C1(C)C=CC=CC=1.C(O)C>[CH:1]1([C:6](=[N:17][OH:18])[CH2:7][N+:8]([O-:10])=[O:9])[CH2:5][CH2:4][CH2:3][CH2:2]1

Participants

4

Reactant 2

HCID 159255Hydroxylamine, sulfate (1:1)HCID 23498804HCID 23498804, compound

Product 1

HCID 74057258HCID 74057258, compoundYield 88.7%

Reagents, catalysts & solvents 1

HCID 21863594Toluene ethanolSolvent

Procedure

9.90 g (63 mmol) of 1-cyclopentyl-2-nitro-ethanone (example II) and 20.688 g (126 mmol) of hydroxylamine sulfate are heated under reflux, for 4 hours, in 310 ml of a toluene/ethanol mixture (1:1). The solvent is removed in vacuo and the residue is taken up in ethyl acetate; the organic phase is washed 2 times with water and dried over sodium sulfate and the solvent is removed in vacuo. 9.62 g (74%) of pale yellow solid are obtained.

Workup

  1. customThe solvent is removed in vacuo
  2. washthe organic phase is washed 2 times with water
  3. dry with materialdried over sodium sulfate
  4. customthe solvent is removed in vacuo

Sources & evidence

ORD record
ord-43cb7551b91042fb94929d115823efe6
Source dataset
uspto-grants-2004_08
Patent number
US06777416B2

Reaction notes

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