2,4Dimethyl2(4methyl3Pentenyl)1,3dioxolane were synthesized with the phosphotungstic acid supported on cationic exchange resin as a catalyst.Various factors that affect the condensation yield were inve...2,4Dimethyl2(4methyl3Pentenyl)1,3dioxolane were synthesized with the phosphotungstic acid supported on cationic exchange resin as a catalyst.Various factors that affect the condensation yield were investigated.The results showed that the optimum conditions were as follows:6methyl5heptene2one:1,2Propandiol:catalyst:dehydrating agent is 1 mol:15mol∶12g∶200ml;reaction temperature was reflux temperature;reaction time was 25h.The yield was above 915% under the optimum conditions.The catalyst can be used repeatedly.展开更多
The selective epoxidation of 3,3-(1,2-ethanediyl-bisoxy)-5(10),9(11)-estradiene-17-α-(1-propynyl)-17-β-ol with Fe(Ⅱ)Pc/PhIO was investigated at 25 ℃? atmospheric pressure. With a molar ratio of Fe(Ⅱ)Pc∶compound...The selective epoxidation of 3,3-(1,2-ethanediyl-bisoxy)-5(10),9(11)-estradiene-17-α-(1-propynyl)-17-β-ol with Fe(Ⅱ)Pc/PhIO was investigated at 25 ℃? atmospheric pressure. With a molar ratio of Fe(Ⅱ)Pc∶compound(I)∶PhIO at 6.25∶50∶120, the conversion reaches 100%. The overall yield of the products 5α, 10α-epoxide(2) and 5β, 10β-epoxide(3)is 60%, and the molar ratio of 2 to 3 is {8.39∶}1. The product 5α, 10α-epoxide is identified by melting point and HPLC.展开更多
以甘油和苯甲醛为原料,对甲苯磺酸为催化剂,制备了甘油苯甲醛缩醛,产物分为2种:4-羟甲基-2-苯基-1,3-二氧戊环(五元环)和2-苯基-1,3-二氧六环-5-醇(六元环)。分别研究了原料摩尔比、带水剂用量、催化剂用量及反应时间对反应的影响。结...以甘油和苯甲醛为原料,对甲苯磺酸为催化剂,制备了甘油苯甲醛缩醛,产物分为2种:4-羟甲基-2-苯基-1,3-二氧戊环(五元环)和2-苯基-1,3-二氧六环-5-醇(六元环)。分别研究了原料摩尔比、带水剂用量、催化剂用量及反应时间对反应的影响。结果表明,在n(甘油)∶n(苯甲醛)=1.2∶1,带水剂体积为15 m L,催化剂质量为0.15 g,反应时间为4 h的较优反应条件下,得到了缩醛产物最大收率为97%(以苯甲醛计)。利用气相色谱(GC)、气相色谱-质谱联用仪(GC-MS)、核磁共振氢谱(1H-NMR)对目标产物进行了定量和定性分析。展开更多
文摘2,4Dimethyl2(4methyl3Pentenyl)1,3dioxolane were synthesized with the phosphotungstic acid supported on cationic exchange resin as a catalyst.Various factors that affect the condensation yield were investigated.The results showed that the optimum conditions were as follows:6methyl5heptene2one:1,2Propandiol:catalyst:dehydrating agent is 1 mol:15mol∶12g∶200ml;reaction temperature was reflux temperature;reaction time was 25h.The yield was above 915% under the optimum conditions.The catalyst can be used repeatedly.
文摘The selective epoxidation of 3,3-(1,2-ethanediyl-bisoxy)-5(10),9(11)-estradiene-17-α-(1-propynyl)-17-β-ol with Fe(Ⅱ)Pc/PhIO was investigated at 25 ℃? atmospheric pressure. With a molar ratio of Fe(Ⅱ)Pc∶compound(I)∶PhIO at 6.25∶50∶120, the conversion reaches 100%. The overall yield of the products 5α, 10α-epoxide(2) and 5β, 10β-epoxide(3)is 60%, and the molar ratio of 2 to 3 is {8.39∶}1. The product 5α, 10α-epoxide is identified by melting point and HPLC.
文摘以甘油和苯甲醛为原料,对甲苯磺酸为催化剂,制备了甘油苯甲醛缩醛,产物分为2种:4-羟甲基-2-苯基-1,3-二氧戊环(五元环)和2-苯基-1,3-二氧六环-5-醇(六元环)。分别研究了原料摩尔比、带水剂用量、催化剂用量及反应时间对反应的影响。结果表明,在n(甘油)∶n(苯甲醛)=1.2∶1,带水剂体积为15 m L,催化剂质量为0.15 g,反应时间为4 h的较优反应条件下,得到了缩醛产物最大收率为97%(以苯甲醛计)。利用气相色谱(GC)、气相色谱-质谱联用仪(GC-MS)、核磁共振氢谱(1H-NMR)对目标产物进行了定量和定性分析。
