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1.c EXAMPLE 1
(c) A mixture of 5.0 g (0.019 mol) of 2-(2-acetyl-3,5-dichlorophenoxy) acetic acid, 10.0 g of anhydrous sodium acetate and 50 ml of acetic anhydride was heated at 155° C. for 0.5 hour. The mixture was poured on to 100 g of ice and 100 ml of a saturated sodium bicarbonate solution. When decomposition of the excess acetic anhydride was complete, the mixture was extracted with three 100 ml portions of diethyl ether. The combined extracts were washed neutral with saturated sodium bicarbonate solution, dried over sodium sulphate and evaporated to give a brown oil which solidified on standing. The crude product was purified by distillation to yield 2.4 g of pure 4,6-dichloro-3-methylbenzofuran of boiling point 85° C./1 mmHg. The distilled product could be crystallized from petrol (boiling point 40°-60° C.) in the form of white needles of melting point 45° C.
5
[ 81078-72-0 ]
3-bromoethyl-4,6-dichlorobenzofuran[ No CAS ]
Yield
Reaction Conditions
Operation in experiment
With N-Bromosuccinimide In tetrachloromethane
1.d EXAMPLE 1
(d) A solution of 2.01 g (0.01 mol) of 4,6-dichloro-3-methylbenzofuran in 50 ml of carbon tetrachloride was treated with 1.79 g (0.1 mol) of N-bromosuccinimide and the mixture was heated under reflux while irradiating with a 200 watt lamp. The reaction was complete after 1.5 hours (determined by thin-layer chromatography). The solution was left to cool and was then filtered. The filtrate was washed with 50 ml of sodium bicarbonate solution, dried over sodium sulphate and evaporated to give a brown oil. The oil was distilled in a Kugelrohr apparatus, to afford a cream colored oil which crystallized on standing (2.2 g). Crystallization from petroleum ether (boiling point 40° C.-60° C.) at 0° C. yielded 3-bromoethyl-4,6-dichlorobenzofuran in the form of cream colored needles of melting point 43° C.
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