反应详情

温度

50 °C

Using the procedure of Example 4, 109 mg of 50% sodium hydride, 510 mg of the product of Example 2 and 4 ml of dimethyl-sulfoxide were reacted and rinsing was carried out with 0.5 ml of dimethylsulfoxide. Then, 20 minutes after the release of hydrogen had stopped, 1.004 g of 3-bromopropoxydiphenyl-tert-butyl-silane were added and the solution was heated to about 50° C. Proceeding as in Example 4, the solution was taken up in 30 ml of methanol, 10 ml of 2N hydrochloric acid, 10 ml of chloroform and refluxed. After purification on silica with methylene chloride-acetone: 8-2 as eluant, 441 mg of the expected product (white crystals) melting at 155°-156° C. were obtained.

1. customwere reacted
2. washrinsing
3. custom20 minutes
4. addition1.004 g of 3-bromopropoxydiphenyl-tert-butyl-silane were added
5. temperature10 ml of 2N hydrochloric acid, 10 ml of chloroform and refluxed
6. customAfter purification on silica with methylene chloride-acetone