Barium Carbonate → HCID 86756305, compound

HRID 567664Notes

Reaction equation

HRID 567664 reaction equation
C[CH:2]1[CH2:6][S:5][CH:4]([C:7]([O:9][CH:10]([CH3:12])[CH3:11])=[O:8])[C:3]1=[O:13].[ClH:14].NO.C(=O)([O-])[O-].[Ba+2]>C(O)(C)C>[Cl:14][CH:2]1[CH2:6][S:5][CH:4]([C:7]([O:9][CH:10]([CH3:12])[CH3:11])=[O:8])[C:3]1=[O:13]

Participants

5

Reactant 3

HCID 10563Barium CarbonateHCID 443297Hydroxyamine hydrochlorideHCID 86756306HCID 86756306, compound

Product 1

HCID 86756305HCID 86756305, compound

Reagents, catalysts & solvents 1

HCID 3776IsopropanolSolvent

Procedure

A mixture of 505 g (2.5 mol) of i-propyl 4-methyl-3-oxo-tetrahydrothiophene-2-carboxylate, 497 g (7.2 mol) of hydroxylamine hydrochloride, 753 g (3.8 mol) of barium carbonate and 2.5 litres of isopropanol is heated under reflux for about 12 hours. The mixture is subsequently filtered off with suction, the filter cake is washed with hot isopropanol and the filtrate is concentrated using water pump vacuum. The residue is taken up in 2 litres of diethyl ether, washed twice with water, dried over magnesium sulphate and filtered. The solvent is carefully distilled off from the filtrate using water pump vacuum.

Workup

  1. temperatureis heated
  2. temperatureunder reflux for about 12 hours
  3. filtrationThe mixture is subsequently filtered off with suction
  4. washthe filter cake is washed with hot isopropanol
  5. concentrationthe filtrate is concentrated
  6. washwashed twice with water
  7. dry with materialdried over magnesium sulphate
  8. filtrationfiltered
  9. distillationThe solvent is carefully distilled off from the filtrate

Sources & evidence

ORD record
ord-8f4ccd81cf5b4b1ab86f03f3741c5b8a
Source dataset
uspto-grants-2001_01
Patent number
US06180567B2

Reaction notes

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