反应详情

After 191.2 g (1.25 mol) of p-nitrobenzyl alcohol is dissolved in 250 ml of methylene chloride, 98.8 g of pyridine is added, and the mixture is cooled to -5° to 0° C. A solution of 193.75 g (1.25 mol) of γ-chloroacetoacetyl chloride (γ-CAC) in 431 ml of methylene chloride is added at the same temperature over an hour and, after completion of the addition, the mixture is stirred for 30 minutes. The resulting pyridine hydrochloride is filtered off. The filtrate and washings are combined and washed with 2 l-portions of water. The organic layer is dried over sodium sulfate and the solvent is then distilled off to give 354 g of p-nitrobenzyl γ-chloroacetoacetate as an oil.

1. temperaturethe mixture is cooled to -5° to 0° C
2. additionafter completion of the addition
3. filtrationThe resulting pyridine hydrochloride is filtered off
4. washwashed with 2 l-portions of water
5. dry with materialThe organic layer is dried over sodium sulfate
6. distillationthe solvent is then distilled off