Sodium Carbonate → HCID 15336967, compound

HRID 1280556Notes

Reaction equation

HRID 1280556 reaction equation
[O:1]1[C:5]2([CH2:10][CH2:9][C:8](=O)[CH2:7][CH2:6]2)[O:4][CH2:3][CH2:2]1.Cl.[NH2:13][OH:14].C(=O)([O-])[O-].[Na+].[Na+]>O>[O:1]1[C:5]2([CH2:10][CH2:9][C:8](=[N:13][OH:14])[CH2:7][CH2:6]2)[O:4][CH2:3][CH2:2]1

Participants

5

Reactant 3

HCID 10340Sodium CarbonateHCID 443297Hydroxyamine hydrochlorideHCID 5674151,4-Dioxaspiro[4.5]decan-8-one

Product 1

HCID 15336967HCID 15336967, compoundYield 397.2%

Reagents, catalysts & solvents 1

HCID 962WaterSolvent

Procedure

To a mixture of 1,4-dioxaspiro[4.5]decan-8-one (50.3 g, 322.1 mmol) and hydroxylamine hydrochloride (89.5 g, 100.3 mmol) in water (450 mL) was added portionwise sodium carbonate (102.4 g, 966.2 mmol). The reaction mixture was stirred for 40 minutes at room temperature then extracted with ethyl acetate. The organic layer was washed with brine, dried over magnesium sulfate, filtered and concentrated in vacuo to give 68.2 g of crude 1,4-dioxaspiro[4.5]decan-8-one oxime.

Workup

  1. extractionthen extracted with ethyl acetate
  2. washThe organic layer was washed with brine
  3. dry with materialdried over magnesium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated in vacuo

Sources & evidence

ORD record
ord-3388ef251a5e44b1ab871854dbb3688d
Source dataset
uspto-grants-2002_09
Patent number
US06451804B1

Reaction notes

Loading…