Hydroxylamine → HCID 178513223, compound

HRID 2388355Notes

Reaction equation

HRID 2388355 reaction equation
[O:1]1[C:5]2([CH2:10][CH2:9][CH:8]([C:11]#[N:12])[CH2:7][CH2:6]2)[O:4][CH2:3][CH2:2]1.[NH2:13][OH:14]>C(O)C>[OH:14][NH:13][C:11]([CH:8]1[CH2:9][CH2:10][C:5]2([O:4][CH2:3][CH2:2][O:1]2)[CH2:6][CH2:7]1)=[NH:12]

Participants

4

Reactant 2

HCID 787HydroxylamineHCID 111164331,4-Dioxaspiro[4.5]decane-8-carbonitrile

Product 1

HCID 178513223HCID 178513223, compound

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

A mixture of 1,4-dioxa-spiro[4.5]decane-8-carbonitrile (0.40 g, 2.4 mmol, prepared according to the procedure from Tremblay, Maxime, PCT Int. Appl. (2007), WO 2007013848) and hydroxylamine (Aldrich, 50% in H2O, 0.7 mL, 9.6 mmol) in ethanol (1.5 mL) in a sealed tube was heated to 80° C. for 6 h. After removal of organic solvent by evaporation, the residue was dissolved in water, extracted with EtOAc and dried over Na2SO4. Filtration and evaporation to dryness gave the product as a white solid.

Workup

  1. customprepared
  2. customAfter removal of organic solvent
  3. customby evaporation
  4. dissolutionthe residue was dissolved in water
  5. extractionextracted with EtOAc
  6. dry with materialdried over Na2SO4
  7. filtrationFiltration and evaporation to dryness

Sources & evidence

ORD record
ord-d90d2d7c770b48e0bb781d73e244f5b9
Source dataset
uspto-grants-2012_09
Patent number
US08269015B2

Reaction notes

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