反应详情

温度

0 °C

Lithium aluminum hydride (190 mL of a 1M ethereal solution) is cooled to 0° C. and treated with aluminum chloride (8.44 g, 63.2 mmol) in 15 mL of diethyl ether. The resulting clear solution is stirred at 0° C. for 20 minutes and then a slurry of tetrahydro-7-(4-methoxyphenyl)-1,4-thiazepin 5-one (15.0 g, 63.2 mmol) in 150 mL of tetrahydrofuran is added. The reaction is then allowed to warm to room temperature for 12 hours and is treated with 14.4 mL of water, 7.2 mL of a 10% aqueous sodium hydroxide solution and 36 mL of water. The mixture is stirred for 3 hours and filtered. The filtrate is concentrated to obtain 8.14 g of a clear oil. The oil is converted to the hydrochloride salt; mp 209°-212° C.

1. temperatureto warm to room temperature for 12 hours
2. stirringThe mixture is stirred for 3 hours
3. filtrationfiltered
4. concentrationThe filtrate is concentrated