反应详情

3-Ethoxypropyl bromide (7.5 g., 0.045 mole) is converted to the Grignard reagent using standard procedures (see above). To this solution (ca 60 ml.), stirred in an ice bath, is added dropwise a solution of 10 g. (0.030 mole) of 3-iodo-5H-dibenzo[a,d]cyclohepten-5-one in 30 ml. of dry THF. The mixture is stirred for 5 minutes and concentrated in vacuo. The residue is treated with saturated ammonium chloride solution and extracted three times with ether. The ether layer is washed once with water, dried over sodium sulfate, and evaporated in vacuo to an orange solid, m.p. 95°-105° (12.0 g., 95%).

1. additionis added dropwise a solution of 10 g
2. stirringThe mixture is stirred for 5 minutes
3. concentrationconcentrated in vacuo
4. additionThe residue is treated with saturated ammonium chloride solution
5. extractionextracted three times with ether
6. washThe ether layer is washed once with water
7. dry with materialdried over sodium sulfate
8. customevaporated in vacuo to an orange solid, m.p. 95°-105° (12.0 g., 95%)