反应详情

A mixture of 9.5 g of 2-acetyl-6,7-dichloro-5-methoxybenzo[b]thiophene and 95 g of pyridine hydrochloride is heated at 185°-200° for four and one-half hours and allowed to cool. While still fluid in nature, the reaction mixture is poured onto ice and the resulting aqueous mixture is extracted three times with ethyl acetate. The organic fractions are combined, washed one time with water, two times with 2N hydrochloric acid, dried over anhydrous magnesium sulfate and evaporated. The residue is recrystallized from acetone-hexane to give 5.1 g of 2-acetyl-6,7-dichloro-5-hydroxybenzo[b]thiophene, mp 199°-201°.

1. temperatureis heated at 185°-200° for four and one-half hours
2. temperatureto cool
3. additionWhile still fluid in nature, the reaction mixture is poured onto ice
4. extractionthe resulting aqueous mixture is extracted three times with ethyl acetate
5. washwashed one time with water, two times with 2N hydrochloric acid
6. dry with materialdried over anhydrous magnesium sulfate
7. customevaporated
8. customThe residue is recrystallized from acetone-hexane