1.

)Requirements for preparation of N-formylbenzotriazole:

Standard procedure.
Simple reaction between the ingredients involves mixing of acetic
anhydride with benzotriazole dissolved in THF under inert atmosphere
(argon supply or nitrogen supply) at very low temp. (20C)
Another procedure
We have: To a mixture of benzotriazole(14.85g) and formic acid(6.9g) in anhydrous
CH2Cl2 (250ml)was added 1,3-dicyclohexylcarbodiimide (36.05g). The mixture was
stirred at r.t for 15h, the precipitate filtered and the solvent removed in vacuo.
Recrystallization of the residue gave pure N-formyl benzotriazole as white needles.
2 . Requirements for 1-aminobenzotriazole:
Benzotriazole dissolved in solution of KOH in water at 60. Solid
hydroxylamine-o-sulphonic acid added in portions during 1hr. temp maintained
70 -75 . Mixture stirred for one hr., cooled, filtered. The alkaline solution was
extracted with ether.
3. Requirements for Hydroxylamine-O-Sulphonic acid:
62 g of bis(hydroxylammonium)sulfate is added to 225g of 30% fuming
H2SO4 .150 ml of anhy . ethyl ether is then added to above solution. Then filtration,
then give washings with ethyl ether.
OR
Reaction between hydroxyl amine and chlorosulphuric acid will result in
formation of desired product.
Chemicals with us
Benzotriazole
Cholorsulphuric acid
THF
Acetic anhydride