DR ALOK KHULLAR,DR INDER KUMAR,DR RAJEEV KUMAR SHARMA,DR SUDHIR KUMAR SHARMA,DR DHANANJAY SRIVASTAVA,DR RANJAN,DR S MADHUSOODANAN
申请号：
IN766/DEL/2002
公开号：
IN2002DE00766A
申请日:
2002.07.23
申请国别(地区):
IN
年份:
2014
代理人:
摘要：
This invention relates to a process for preparing Deltamethrin comprising: preparing Delta-3-Caren-5-one by oxidizing Delta-3- Carene in the presence of air/oxygen and cobalt pyridinium halide catalyst and subsequently isolating Delta-3-Caren-5-one through continuous distillation and fractionation at 0.5-1.0 mm. Hg subjecting the said Delta-3-Caren-5-one in a polar/non-polar solvent to ozonolysis at -5 to -12�C followed by quenching with aqueous sodium sulfite solution to obtain crude C9-Ketoacid in a known manner, purifhying the said C9-Ketoacid chemically by forming alkali metal salt of the said acid, extracting out the non-acidic impurities with a water immiscible polar / non-polar solvent and isolating the purified C9-Ketoacid by acidification with aqueous mineral acid, followed by extraction with a water immiscible polar/non-polar solvent and finally stripping off the said polar/non-polar solvent under reduced pressure (60-70�C/50-200mm. Hg), stirring the said purified Cg-Ketoacid with an acid anhydride (1.0-1.5 mole w.r.t. C9-Ketoacid) and para-toluene sulphonic acid catalyst (PTSA, 4-5 mole percent w.r.t. C9-Ketoacid) at 15�5�C until lactonisation is complete, adding an alkali metal acetate in pre-determined quantity to neutralize PTSA and distilling off the acid along with un-reacted acid anhydride under reduced pressure (70-90�C/60-90 mm. Hg), extracting the residual mass with a water immisicible polar / non-polar solvent and washing off the acidic impurities with aqueous alkali metal carbonate/bi-carbonate solution, isolating the crude C9-Enol lactone by removal of the said polar / non-polar solvent xmder reduced pressure (60-70�C/50-200 mm. Hg) and purifying it by distillation under reduced pressure (68-70�C/1.0 mm. Hg), subjecting the said C9-Enol lactone to ozonolysis in polar/non-polar solvent, followed by quenching the reaction mass, atjow temperature, with an alcoholic or aqueous solution of a reducing agent that gets easily oxidized un
