Title of Invention

"A PROCESS FOR THE PREPARATION OF N-HENEICOSANE"

Abstract This invention relates to a process for the preparation of n-heneicosane which comprises reacting 5 to 9 wt % 2,4-alkanedione with 45 to 55 wt % of 1-bromooctadecane in 20 to 40 wt % absolute ethanol in the presence of 0.005 to 0.009 wt % 18-crown-6 catalyst, refluxed at 80-100°C with continuous string for 24-42 hrs to produce 2-heneicosanone; reducing said 2-heneicosanone by refluxing at 90-130°C with continuous stirring for 4-8 hrs with a mixture of 8 to 15 wt% hydrazine hydrate and 10 to 15 wt % of potassium hydroxide pellets in 55 to 70 wt% diethylene glycol or Triethylene glycol, followed by removal of water and excess hydrazine from the said mixture by distillation and further refluxing the said mixture at 200-300°C for 8-16 hrs to obtain n-heneicosane.
Full Text


WE CLAIM:
1. A process for the preparation of n-heneicosane which comprises:-
(c) reacting 5 to 9 wt % 2,4-alkanedione with 45 to 55 wt % of 1-bromooctadecane in 20 to 40 wt % absolute ethanol in the presence of 0.005 to 0.009 wt % 18-crown-6 catalyst, refluxed at 80-100°C with continuous string for 24-42 hrs to produce 2-heneicosanone;
(d) reducing said 2-heneicosanone by refluxing at 90-130°C with continuous stirring for 4-8 hrs with a mixture of 8 to 15 wt% hydrazine hydrate and 10 to 15 wt % of potassium hydroxide pellets in 55 to 70 wt% diethylene glycol or Triethylene glycol, followed by removal of water and excess hydrazine from the said mixture by distillation and further refluxing the said mixture at 200-300°C for 8-16 hrs to obtain n-heneicosane.

2. A process as claimed in claim 1, wherein said 2, 4-alkanedione is selected from 2,4-propanedione and 2,4-pentanedione.
3. A process as claimed in claim 1, wherein the amount of said 2,4-alkanedione is preferably 7 to 8 wt%, the amount of said 1-bromooctadecane is preferably 48 to 52 wt%, the amount of said 18-crown_6 is preferably 0.006 to 0.008 wt %, the amount of said anhydrous potassium carbonate is preferably 11 to 12% and the amount of said absolute ethanol is preferably 28 to 32 wt%.
4. A process as claimed in any preceding claim, wherein in step (a), the reactants are refluxed at preferably 85-95 °C with continuous stirring for preferably 30-36 hrs.
5. A process as claimed in any preceding claim, wherein said ethylene glycol
is selected from diethylene glycol and triethylene glycol.
6. A process as claimed in any preceding claim, wherein the said step (b) is
carried out by refluxing 2-heneicosanone obtained in step (a) with a
mixture of preferably 10 to 12 wt% of hydrazine hydrate, preferably 11 to
13 wt% of potassium hydroxide pellets and preferably 60 to 65 wt%
diethylene glycol or triethylene glycol.
7. A process as claimed in claim 6, wherein said refluxing instep (b) is carried out at preferably 110-120 °C with continuous stirring for preferably 6-8 hrs, and further refluxing said mixture at elevated temperature of preferably 210-220 °C preferably for 11-13 hrs.

Documents:

418-DEL-2005-Abstract-(31-10-2011).pdf

418-del-2005-abstract.pdf

418-DEL-2005-Claims-(31-10-2011).pdf

418-del-2005-Correspondence Others-(02-06-2011).pdf

418-del-2005-Correspondence Others-(09-05-2011).pdf

418-DEL-2005-Correspondence Others-(15-07-2011).pdf

418-DEL-2005-Correspondence Others-(31-10-2011).pdf

418-del-2005-correspondence-others.pdf

418-del-2005-correspondence-po.pdf

418-del-2005-description (complete).pdf

418-DEL-2005-Form-1-(31-10-2011).pdf

418-del-2005-form-1.pdf

418-del-2005-form-13.pdf

418-del-2005-form-18.pdf

418-del-2005-form-2.pdf

418-DEL-2005-Form-3-(31-10-2011).pdf

418-del-2005-form-3.pdf

418-del-2005-GPA-(02-06-2011).pdf

418-DEL-2005-GPA-(31-10-2011).pdf

418-del-2005-gpa.pdf

418-DEL-2005-Petition-137-(31-10-2011).pdf


Patent Number 253005
Indian Patent Application Number 418/DEL/2005
PG Journal Number 25/2012
Publication Date 22-Jun-2012
Grant Date 14-Jun-2012
Date of Filing 25-Feb-2005
Name of Patentee THE DIRECTOR GENERAL DEFENCE RESEARCH AND DEVELOPMENT ORGANIZATION
Applicant Address MINISTRY OF DEFENCE, GOVERNMENT OF INDIA, WEST BLOCK-VIII, WING-I, SECTOR-1, R.K.PURAM, NEW DELHI-110 066
Inventors:
# Inventor's Name Inventor's Address
1 KUMARAN GANESAN DEFENCE RESEARCH & DEVELOPMENT ESTABLISHMENT, JHANSI ROAD, GWALIOR-474 002, MADHYA PRADESH, INDIA
2 RAMESH CHANDRA MALHOTRA DEFENCE RESEARCH & DEVELOPMENT ESTABLISHMENT, JHANSI ROAD, GWALIOR-474 002, MADHYA PRADESH, INDIA
3 AMBATI NARASIMHA RAO DEFENCE RESEARCH & DEVELOPMENT ESTABLISHMENT, JHANSI ROAD, GWALIOR-474 002, MADHYA PRADESH, INDIA
4 PRADEEP KUMAR GUPTA DEFENCE RESEARCH & DEVELOPMENT ESTABLISHMENT, JHANSI ROAD, GWALIOR-474 002, MADHYA PRADESH, INDIA
5 ASHEESH KUMAR JAIN DEFENCE RESEARCH & DEVELOPMENT ESTABLISHMENT, JHANSI ROAD, GWALIOR-474 002, MADHYA PRADESH, INDIA
6 SHRI PRAKASH DEFENCE RESEARCH & DEVELOPMENT ESTABLISHMENT, JHANSI ROAD, GWALIOR-474 002, MADHYA PRADESH, INDIA
7 KRISHNAMURTHY SEKHAR DEFENCE RESEARCH & DEVELOPMENT ESTABLISHMENT, JHANSI ROAD, GWALIOR-474 002, MADHYA PRADESH, INDIA
PCT International Classification Number C07C 9/12
PCT International Application Number N/A
PCT International Filing date
PCT Conventions:
# PCT Application Number Date of Convention Priority Country
1 NA