Dimethyl butyric acid is added into a reactor and phosphorus trichloride is added while stirring; then the mixture is heated to react; the mixture is cooled to room temperature after reaction and then is kept still for delamination; after delamination, orthophosphorous acid at the lower layer is regarded as byproduct, and acyl chloride crude product at the upper layer is distillated under absolute pressure 20KPa through reduced pressure distillation and the distillate at 79-81 DEG C is collected; in this way, 3, 3-dimethyl butyric acid chloride can be obtained.
向反应器中加入3，3-二甲基丁酸，搅拌，加入三氯化磷，升温至反应温度进行反应，反应结束后冷却至室温并静置分层；将静置分层后分出下层的亚磷酸，作为副产品，取上层的酰氯粗品在绝对压力20KPa下经减压蒸馏收集79～81℃的馏分，即得到3，3-二甲基丁酰氯产品。