1-butylazepan-2-one

反应条件: temp:150.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 113.2 g of fresh caprolactam (1.0 mol) is dissolved in 250 g of crude distillate containing 3.4% of caprolactam (8.5 g of caprolactam prepared as in a), and the resulting mixture is heated to 150° C. 202 g of a 30.16 wt. % strength sodium methoxide-methanol solution (1.13 mol) is metered in at 140° C. over a period of one hour while distilling methanol. All the methanol is distilled by briefly applying vacuum. 104.5 g of n-butyl chloride (1.13 mol) is then metered in at 140° C. over a period of one hour. After allowing the mixture to continue reacting for 4 hours, the reaction mixture is subjected to an initial cooling, and all the NBC is distilled from the sodium chloride in vacuo; boiling point of NBC: 90° C./0.5 mbar. Weight: 406 g. GC Purity: 96.3% of NBC, 2.7% of caprolactam. Yield: 83.0% of theory or 91.2% if caprolactam is recycled. NBC can be redistilled through a column to give a product having a purity of about 99%. prepared as in a), and the resulting mixture while distilling methanol All the methanol is distilled an initial cooling all the NBC is distilled from the sodium chloride in vacuo 90° C./0.5 mbar NBC can be redistilled through a column to give a product