反应详情

The ether XXVI (213 g, 0.79 mole) at 25°C was stirred as 0.9 M lithium aluminum hydride in diethylene glycol diethyl ether (484 ml, 0.436 mole of Li Al H4) was added dropwise. Then the product was distilled at atmospheric pressure through a cold water condensor into an ice cooled receiver until 157 g of IV was collected. This distillate was fractionally distilled to give IV, b760 68.1°-68.2°C, of 99.7% purity (by gas-liquid chromatography) in 93% of the theoretical yield; density at 23°C was 1.554. The structure of IV was confirmed by proton NMR spectroscopy.

1. additionwas added dropwise
2. distillationThen the product was distilled at atmospheric pressure through a cold water condensor into an ice cooled receiver until 157 g of IV
3. customwas collected
4. distillationThis distillate was fractionally distilled