Hydrochloric Acid → HCID 18322312, compound

HRID 1698849Notes

Reaction equation

HRID 1698849 reaction equation
Cl.[NH2:2][OH:3].[OH-:4].[Na+].[CH2:6]([CH:8]([C:15](=O)[CH2:16][CH2:17][CH3:18])[CH2:9]C(OCC)=O)[CH3:7].Cl>O>[CH2:6]([C:8]1[C:9](=[O:4])[O:3][NH:2][C:15]=1[CH2:16][CH2:17][CH3:18])[CH3:7]

Participants

6

Reactant 4

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 443297Hydroxyamine hydrochlorideHCID 10867342HCID 10867342, compound

Product 1

HCID 18322312HCID 18322312, compound

Reagents, catalysts & solvents 1

HCID 962WaterSolvent3×

Conditions

Temperature
50 °C

Procedure

11.53 g (165.9 mmol) of hydroxylamine hydrochloride are dissolved in 25 ml of water and, at a temperature of at most 0°C., admixed with a solution of 13.27 g (331.8 mmol) of sodium hydroxide in 60 ml of water. Without further cooling, 30.9 g (165.9 mmol) of ethyl 2-ethylhexan-3-onecarboxylate are then added in one portion, and the mixture is stirred at 50° C. for 3 h. For work-up, 15.5 ml of conc. hydrochloric acid are added at 0°C., and the mixture is diluted with water and extracted three times with dichloromethane. The organic phase is dried over sodium sulphate, concentrated and fractionated under high vacuum. B.p.2mbar 105-115°C.

Workup

  1. extractionextracted three times with dichloromethane
  2. dry with materialThe organic phase is dried over sodium sulphate
  3. concentrationconcentrated
  4. customB.p.2mbar 105-115°C.

Sources & evidence

ORD record
ord-8a98e6a2e91e4e60bcf8654cba8235b4
Source dataset
uspto-grants-2002_02
Patent number
US06344471B1

Reaction notes

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