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A STUDY ON THE CATALYTIC ACTIVITY OF THE

ZEOLITE ZSM-5 IN HETEROGENEOUS PHASE

Mr. Balin Kumar Bhuyan

Department of Chemistry, Gauhati University, Guwahati-781014, Assam

The thesis entitled A STUDY ON THE CATALYTIC ACTIVITY OF THE

ZEOLITE ZSM-5 IN HETEROGENEOUS PHASE includes six chapters as

follows.

1. Introduction

2. Synthesis and characterisation of Ti-ZSM-5

3. Ti-exchanged ZSM-5 as heterogeneous catalyst for

allylation of aldehydes with allyltributylstannane

4. Acetylation of various alcohols using Ti-ZSM-5 as catalyst

5. Oxidation of alcohols and carbonyl compounds using Ti-ZSM-5 as

catalyst .

6. Mukaiyama aldol reaction of ketene silyl acetals with aldehyde catalyzed

by Ti-ZSM-5

CHAPTER I

INTRODUCTION

Chapter I gives a general introduction about the zeolite emphasizing its

wide scientific interest as a solid acid catalyst. This chapter describes briefly

the definition, structure, nomenclature, classification and properties of the

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zeolites. The applications of zeolites in various fields are highlighted with a

special reference to ZSM-5. Some shape selective reactions and a few ZSM-5

catalysed reactions studied so far have been incorporated in this chapter with

references.

CHAPTER II

SYNTHESIS AND CHARACTERISATION OF Ti-ZSM-5

Chapter II gives a brief description of chronological development in the history

of zeolite synthesis science so far. Parameters influencing zeolite synthesis

and modification of zeolites by metal substitution are also discussed. An

efficient method of incorporation of Titanium in ZSM-5 by ion-exchange is

included in this chapter. Characterisations of the various samples of

synthesized Ti-ZSM-5 by different analytical techniques such as X-ray Powder

diffraction, FTIR spectroscopy. SEM, EDX analysis and UV-VIS spectroscopy

are described and analyses are given.

CHAPTER III

Ti-exchanged ZSM-5 as heterogeneous catalyst for allylation

of aldehydes with allyltributylstannane

The addition of allyl metal reagents to aldehydes is an important method for

formation of carbon-carbon bond. Allyltributylstannane is one of the most

common reagents used for the synthesis of homoallylic alcohols. A method

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has been described in this chapter, for the synthesis of homoallylic alcohols

using Ti-exchanged ZSM-5 as heterogeneous catalyst (Scheme 1).

O

R H

SnBu3 Ti-ZSM

Toluene, r.t. R

OH

+-5

Scheme 1

CHAPTER IV

ACETYLATION OF VARIOUS ALCOHOLS USING Ti-ZSM-5

AS CATALYST

The acetylation of alcohols occupies an important role in organic

synthesis and biochemistry. Conventional acetylations have been carried out

by using homogeneous acid or base catalysts. In order to overcome the

difficulties associated with homogeneous catalysts the development and

utilization of solid catalysts are important. This chapter deals with the catalytic

evaluation of Ti-ZSM-5 as heterogeneous catalyst for the acetylation of

alcohols (Scheme 2).

OHOAcAc2O

Ti-ZSM-5,room temp

Scheme 2

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CHAPTER V

OXIDATION OF ALCOHOLS WITH AQUEOUS TBHP INPRESENCE OF Ti-ZSM-5 AS CATALYST.

Since the first synthesis of TS-1 by Tarramasso et al. in 1983, TS-1 has

attracted much attention for its unique catalytic oxidation properties, especially

in selective oxidation reactions under mild conditions. In this chapter, oxidation

reactions have been investigated for certain secondary alcohols and benzyl

alcohols with aqueous tert-butyl hydroperoxide as oxidant in presence of Ti-

ZSM-5 as catalyst. (scheme 3).

OH

Ti-ZSM

TBHP,MeOH

O

5

scheme 3

CHAPTER VI

MUKAIYAMA ALDOL REACTION OF KETEN SILYL ACETALSWITH ALDEHYDE CATALYZED BY Ti-ZSM-5

Mukaiyama aldol reaction is an efficient methodology of carbon-carbon bond

formation reaction. Both Lewis acids and bases are known to catalyze this

reaction. Various metal compounds have been developed to catalyse

Mukaiyama aldol reaction.

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This chapter presents an investigation on the catalytic activity of Ti-

ZSM-5 for Mukaiyama aldol reaction of silyl keten acetal with various

aldehydes. (Scheme 4).

R-CHOOTMS

OMeOMe

OHO

+Ti-ZSM-5 , DMF

Scheme 4

5