反应详情

A mixture of 3-n-butylthio-4-phenoxy-5-sulfamylbenzoic acid (2.3 g), chloroacetonitrile (1.4 g), triethylamine (0.61 g), and dry acetone (20 ml) is refluxed for 20 hours. After cooling the triethylamine hydrochloride formed is removed by filtration, and the filtrate is evaporated in vacuo. To the residue, water (35 ml) and ethylacetate (75 ml) are added, and the pH of the aqueous layer is adjusted to pH 7.5 by addition of 4 N hydrochloric acid. The organic layer is then separated, washed with diluted sodium hydrogen carbonate, dried and evaporated in vacuo. The residue is crystallized from chloroform petroleum ether to yield cyanomethyl 3-n-butylthio-4-phenoxy-5-sulfamylbenzoate with a melting point of 134°-135°C.

1. temperatureis refluxed for 20 hours
2. customformed
3. customis removed by filtration
4. customthe filtrate is evaporated in vacuo
5. additionTo the residue, water (35 ml) and ethylacetate (75 ml) are added
6. additionthe pH of the aqueous layer is adjusted to pH 7.5 by addition of 4 N hydrochloric acid
7. customThe organic layer is then separated
8. washwashed with diluted sodium hydrogen carbonate
9. customdried
10. customevaporated in vacuo
11. customThe residue is crystallized from chloroform petroleum ether