正交试验法优化合成环己酮Vc缩酮

Optimized synthesis of cyclohexanone L-ascorbic acid ketal by orthogonal experiment

Cyclohexanone L-ascorbic acid ketal is synthesized from the reaction of L-isoascorbic acid and cyclohexanone with p-toluene sulfonic acid as catalyst,N,N-dimethyl acetamide(DMAc) as solvent and cyclohexane as water carrying agent.The optimal reaction conditions determined by orthogonal experiment are as follows:L-ascorbic acid 1.76 g(10 mmol),cyclohexanone 1.57 g(16 mmol),p-toluene sulfonic acid 0.38 g(2 mmol),DMAc 6 mL,cyclohexane 9 mL,reaction temperature 120～125℃ and reation time 2.5 h.The yield is 85.8% under these optimal conditions.The title compound is characterized by 1H NMR,FTIR and EI-MS.

Cyclohexanone L-ascorbic acid ketal is synthesized from the reaction of L-isoascorbic acid and cyclohexanone with ptoluene sulfonic acid as eatalyst,N,N-dimethyl acetamide（DMAe） as solvent and cyclohexane as water carrying agent. The optimal reaction conditions determined by orthogonal experiment are as follows ：L-ascorbic acid 1.76 g（ 10 mmol）, eyclohexanone 1.57 g （16 retool）,p-toluene sulfonic acid 0. 38 g（2 mmol）, DMAc 6 mL, eyelohexane 9 mL, reaction temperature 120 ～ 125℃ and reation time 2. 5 h. The yield is 85.8% under these optimal conditions. The title compound is characterized by ^1H NMR, FTIR and EI-MS.