Process Demonstration

Venue: Pilot Plant-II, IICT,Hyd.

Date: 11, Dec,2010

Process: Dye Z907

Process Demo By IICT, Hyderabad.

Client:M/s Sapala Organics(P)Ltd,Hyderabad.

Raw materials used:

1. RuCl3.3H2O 100g

2.α-TERPENINE 620ML

3.Abs Ethanol 14.5 L

4. Di Nonyl Bipyridine 100g

5.DMF 11.5 L

6.DMF 11.5 L

7.Ammonium thiocyanate 290g

8. Deionised water 38 L

9.Hexane 1L

10.DCM 300 L

11.Methanol 300 L
Demo Steps: (Z-907)9.00AM On Dt: 11-12-2010

1. 6 liters of ethanol, 100 grams of RuCl3.3H2O and 620 ml of α-Terpinine are loaded into 20

liter Autoclave (M.C. S.S316) and heated to 800C under stirring .Then maintained this at

800C for 4hr 30 min under N2 blanketing.

2. Now bring down the temperature from 800C to room temperature by stopping heating under

stirring and N2 blanketing. It task one hour.

3. The reactants are then taken in flask and kept in fridge (4oC) for 15 hours to precipitate .

4. Next day (12th Dec, 2010), it is taken out and filtered on WHATMANN filter paper -1 which

took 3hour 10 min .The ethanol collected was 5.8 liter.Then it is washed with hexane (1liter)

taking 30 min and hexane collected from bottom was 950 ml.

5. The precipitate collected on filter paper was kept in desiccator for drying for 3hr 40min

under vacuum .After drying ,the powder collected was 110g.

6. 75 g of Ru -p- cymene complex is along with 8 liters of ethanol are loaded into Auto clave

and 100 g of Di Nonyl Bipyridine is added under stirring and N2 blanketing then heated to

800C.This took 30 min .Then it is maintained for 4 hours and then cooled to RT by cutting

off heating under stirring which took 40 minutes.

7. Next day (13th Dec, 2010),material from autoclave 6 is taken to rotavapour (20 liter) and

solvent is removed by maintaining the temp at 400C and full vacuum, which took 2 hours.

Solvent collected was 7.75 liter.

8. 11.5 liter of DMF and 58.2 g of BI pyridine di carboxylic acid are added in the autoclave and

heated to 120oC with N2 blanketing and stirring. This took 1hr 30 min for complete
 desolution.

9. 1.5 liter of DMF is added to the material in rotavapor.Complete desolution was observed in

30 minutes.

10. The solution from rotavapor is taken into flask and fed into autoclave material at 120°C.

Then the temperature to 153° - 154°C with reflux arrangement. This took 15 minutes to

reach the temperature of 153°-154°C from 120°C. Then maintained this for 4 hours with

stirring and reflux. Then it is brought to 90°C (in 45 minutes). A sample is taken and tested

for UV spectra which matched with standard spectra (Sample – 1).

11. Next day (14th Dec, 2010) ammonium thiocyanate (290 grams) is taken in a flask and 250

ml of deionized water is added with shaking. This dissolved very easily and then

transferred to autoclave at 90°C.Then the temperature is raised to 110°C which took 15

minutes. Then the same is maintained for two hours.

12. After 2 hours, sample is drawn and checked for UV spectra which matched with standard

spectra (Sample – 2).

13. Then the contents of autoclave are cooled to room temperature (35°C) and transferred to 20

liters rotavapour. The solvent is removed (12.75 liters) under vacuum and 53°C

temperature which took five and half hours.

14. It is cooled to room temperature (30 minutes) and then 13 liters of deionized water is added

and run for 30 minutes. Then the flask is kept in fridge (4°C) over night for precipitation.

15. Next day (15th Dec, 2010), it is taken out and filtered on whatman-1 filter paper which took

6 hours collecting 12.8 liters of water.

16. Then the solid on the filter paper was given water wash with 12 liters in 5 hours. Then the

solid material is collected from filter paper and dried in desiccator under vacuum for 10

hours.
17. Next Day (16th Dec, 2010), the crude material collected after drying was 193.4 grams and

sample is tested for UV spectra which matched with standard spectra (Sample – 3). Also

tested for purity on NMR

18. The crude material was purified on sephadex column (2 kg of sephadex) after dissolving it

in a mixture of DCM : Methanol (50:50), i.e., 500 ml DCM amd 500 ml of Methanol.

19. The first band of impurities have been collected at the end of one hour and kept separately.

20. The second band was collected after 3 hours of first band and sample was tested for UV

spectra and it matched with standard spectra (Sample – 4).

21. The second band collected after meeting the purity was taken to rotavapour and run for 3

hours under vacuum to remove Methanol and DCM by maintaining 30°C. The DCM and

methanol was totally recovered (99%).

22. Then the dried product collected from desiccator was 103 grams. It has been further

analyased by NMR and UV spectra. The spectra are enclosed.