SYNTHESIS OF S-BENZYLISOTHIOURONIUM CHLORIDE
- Dissolve 76g (1 mol) of thiourea in 200 ml of warm water in
a 1-litre round-bottomed flask.
- Dilute the solution with 135 ml of rectified
spirit and add 126.5g (1 mol) of benzyl chloride.
- Heat the mixture under
reflux on a water bath until the benzyl chloride dissolves (about 15 minutes)
and for a further 30 minutes taking care that the mixture is well shaken from
time to time.
- Cool the mixture in ice: there is a tendency to supersaturation
so that it is advisable to stir (or shake) the cold solution vigorously, when
the substance crystallises suddenly.
- Filter off the solid at the pump.
- Evaporate the filtrate to about half bulk in order to recover a further small
quantity of product.
- Dry the compound upon filter paper in the air. The yield
of S-benzylisothiouronium chloride, m.p. 174 °C, is 200g (99%).
- Recrystallise
the salt from 400 ml of 0.2 m hydrochloric acid; filter off the solid which
separates on cooling. The yield of recrystallised salt, m.p. 175 °C, is 185g
(91%); some of the dimorphic form, m.p. 150 °C, may also separate.
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