角黄素合成新工艺

New process for canthaxanthin synthesis

1,3-二双键十五碳膦酸酯直接缩合法合成β-胡萝卜素,β-胡萝卜素选择性催化氧化合成角黄素.用单因素实验、均匀实验设计和单纯形寻优法研究β胡萝卜素催化氧化工艺.1,3-二双键十五碳膦酸酯和2,7二甲基2,4,6辛三烯1,8二醛缩合合成β-胡萝卜素,收率68%;催化氧化反应合适工艺条件:β-胡萝卜素6.8g,复合催化剂0.45g,二氯甲烷250ml,饱和次氯酸钠溶液50ml,CO2作酸碱调节剂和惰性气体,-5℃下反应40min,角黄素收率89.6%.β-胡萝卜素和角黄素粗产物用重结晶方法提纯.

A new process for selective catalytic oxidation of β-carotene was proposed. Optimum oxidation conditions were determined by uniform test design and simplex optimization. β-Carotene was synthesized from 3-methyl-5-（2, 6, 6-trimethyl-1-cycolhex-en-1-yl）-1, 3-pentadienylphosphonates and 2, 7 dimethyl- 2,4,6-octatriene-l,8-dial with a yield of 68%. Proper catalytic oxidation conditions were： β carotene 6.8 g, compounded catalyst 0.45 g, dichloromethane 250 ml, saturated sodium hypochlorite 50 ml and reaction temperature -5℃. Carbon dioxide was used to maintain a weak acidic system. The process was completed in 40 min. Purification of β-carotene and canthaxanthin was made by recrystallization.