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由3.5.5——三甲基己醇,经加压混合碱熔制得的3.5.5——三甲基己酸(0.24克分子)和三氯化磷(0.24克分子)于60℃反应三小时,生成3.5.5——三甲基己酰氯。此酰氯(0.198克分子)和34％H_2O_2(0.81克分子)、10％NaOH(0.42克分子)于0——10℃反应150分钟,生成引发剂“K”。以酸为基准的产率为82.26％。产品经化学分析其纯度为96-98％,红外光谱鉴定除含少量杂质(酰氯水解产物)外,和日本CP-10标样图谱一致。
Reaction of 3.5.5-trimethylhexanoic acid (0.24 mol) made with 3.5.5-trimethylhexanol, pressurized mixed alkali melt and phosphorus trichloride (0.24 mol) at 60 ° C Three hours to generate 3.5.5 - trimethylhexanoyl chloride. The acid chloride (0.198 mol) and 34% H 2 O 2 (0.81 mol) and 10% NaOH (0.42 mol) were reacted at 0 - 10 ° C for 150 minutes to form initiator “K”. The acid-based yield was 82.26%. The purity of the product was 96-98% by chemical analysis. The infrared spectroscopy was consistent with the Japan CP-10 standard except for the small amount of impurities (acid chloride hydrolysates).