反应详情

19.7 G. of dibenzo[b,e]thiepin-11(6H)-one and 14.6 g. of hydroxylamine hydrochloride in 350 ml. of pyridine are stirred under reflux conditions for 16 hours. After the addition of a further 7.3 g. of hydroxylamine hydrochloride, the mixture is stirred for a further 5 hours under reflux conditions. The mixture is evaporated and purified by chromatography over aluminum oxide using chloroform and chloroform/methanol (93:3) for the elution. The purified product is recrystallized from acetone. There is obtained dibenzo[b,e]thiepin-11(6H)-one-oxime of melting point 241°-243° C.

1. additionAfter the addition of a further 7.3 g
2. customThe mixture is evaporated
3. custompurified by chromatography over aluminum oxide
4. washfor the elution
5. customThe purified product is recrystallized from acetone