反应详情

A mixture of 2.49 g. (15 mmole) of 2.3-Dihydro-7-methoxy-6-benzofuranol, 5.87 g. (50 mmole) zinc cyanide and 100 ml. of dry ether was saturated with hydrogen chloride for 1 hour at 0°, then for 2 hours at room temperature. The mixture was then allowed to stand overnight at room temperature then concentrated in vacuo and the residue treated with 100 ml. of 0.1N HCl for 1 hour at reflux. After cooling, ether extraction provided the product which was purified by chromatography over silica gel (E. Merck 60), eluting with CHCl3, to yield a colorless solid, m.p. 71°-72°.

1. additionA mixture of 2.49 g
2. waitto stand overnight at room temperature
3. concentrationthen concentrated in vacuo
4. additionthe residue treated with 100 ml
5. temperatureof 0.1N HCl for 1 hour at reflux
6. temperatureAfter cooling
7. extractionether extraction
8. customprovided the product which
9. customwas purified by chromatography over silica gel (E. Merck 60)
10. washeluting with CHCl3
11. customto yield a colorless solid, m.p. 71°-72°