CN113816841A - 一种环丙基甲基酮的制备方法 - Google Patents
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- HVCFCNAITDHQFX-UHFFFAOYSA-N 1-cyclopropylethanone Chemical compound CC(=O)C1CC1 HVCFCNAITDHQFX-UHFFFAOYSA-N 0.000 title claims abstract description 29
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- 238000006243 chemical reaction Methods 0.000 claims abstract description 61
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- XVRIEWDDMODMGA-UHFFFAOYSA-N 5-chloropentan-2-one Chemical compound CC(=O)CCCCl XVRIEWDDMODMGA-UHFFFAOYSA-N 0.000 claims abstract description 35
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- 238000000034 method Methods 0.000 claims abstract description 16
- UAGJVSRUFNSIHR-UHFFFAOYSA-N Methyl levulinate Chemical compound COC(=O)CCC(C)=O UAGJVSRUFNSIHR-UHFFFAOYSA-N 0.000 claims abstract description 13
- 229910000033 sodium borohydride Inorganic materials 0.000 claims abstract description 11
- 239000012279 sodium borohydride Substances 0.000 claims abstract description 11
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims abstract description 11
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims abstract description 9
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims description 30
- JOXIMZWYDAKGHI-UHFFFAOYSA-N toluene-4-sulfonic acid Chemical compound CC1=CC=C(S(O)(=O)=O)C=C1 JOXIMZWYDAKGHI-UHFFFAOYSA-N 0.000 claims description 20
- 239000012043 crude product Substances 0.000 claims description 19
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 15
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 10
- 239000002274 desiccant Substances 0.000 claims description 10
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- 229940017219 methyl propionate Drugs 0.000 claims description 10
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
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- 238000001816 cooling Methods 0.000 claims description 5
- 238000001914 filtration Methods 0.000 claims description 5
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- 238000012544 monitoring process Methods 0.000 claims description 5
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- 238000004821 distillation Methods 0.000 claims description 3
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- 238000009776 industrial production Methods 0.000 abstract description 7
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- 125000002915 carbonyl group Chemical group [*:2]C([*:1])=O 0.000 description 3
- 239000012159 carrier gas Substances 0.000 description 3
- 150000002431 hydrogen Chemical class 0.000 description 3
- 230000014759 maintenance of location Effects 0.000 description 3
- 125000001434 methanylylidene group Chemical group [H]C#[*] 0.000 description 3
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- UFNOUKDBUJZYDE-UHFFFAOYSA-N 2-(4-chlorophenyl)-3-cyclopropyl-1-(1H-1,2,4-triazol-1-yl)butan-2-ol Chemical compound C1=NC=NN1CC(O)(C=1C=CC(Cl)=CC=1)C(C)C1CC1 UFNOUKDBUJZYDE-UHFFFAOYSA-N 0.000 description 1
- HDKKRASBPHFULQ-UHFFFAOYSA-N 3-Hydroxy-2-pentanone Chemical compound CCC(O)C(C)=O HDKKRASBPHFULQ-UHFFFAOYSA-N 0.000 description 1
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- XPOQHMRABVBWPR-UHFFFAOYSA-N Efavirenz Natural products O1C(=O)NC2=CC=C(Cl)C=C2C1(C(F)(F)F)C#CC1CC1 XPOQHMRABVBWPR-UHFFFAOYSA-N 0.000 description 1
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- HAORKNGNJCEJBX-UHFFFAOYSA-N cyprodinil Chemical compound N=1C(C)=CC(C2CC2)=NC=1NC1=CC=CC=C1 HAORKNGNJCEJBX-UHFFFAOYSA-N 0.000 description 1
- XPOQHMRABVBWPR-ZDUSSCGKSA-N efavirenz Chemical compound C([C@]1(C2=CC(Cl)=CC=C2NC(=O)O1)C(F)(F)F)#CC1CC1 XPOQHMRABVBWPR-ZDUSSCGKSA-N 0.000 description 1
- 229960003804 efavirenz Drugs 0.000 description 1
- UWKQSNNFCGGAFS-XIFFEERXSA-N irinotecan Chemical compound C1=C2C(CC)=C3CN(C(C4=C([C@@](C(=O)OC4)(O)CC)C=4)=O)C=4C3=NC2=CC=C1OC(=O)N(CC1)CCC1N1CCCCC1 UWKQSNNFCGGAFS-XIFFEERXSA-N 0.000 description 1
- 229960004768 irinotecan Drugs 0.000 description 1
- 125000001570 methylene group Chemical group [H]C([H])([*:1])[*:2] 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- 238000007363 ring formation reaction Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
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- C07C45/00—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds
- C07C45/61—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by reactions not involving the formation of >C = O groups
- C07C45/65—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by reactions not involving the formation of >C = O groups by splitting-off hydrogen atoms or functional groups; by hydrogenolysis of functional groups
- C07C45/66—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by reactions not involving the formation of >C = O groups by splitting-off hydrogen atoms or functional groups; by hydrogenolysis of functional groups by dehydration
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- C07C45/56—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds from heterocyclic compounds
- C07C45/57—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds from heterocyclic compounds with oxygen as the only heteroatom
- C07C45/59—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds from heterocyclic compounds with oxygen as the only heteroatom in five-membered rings
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- C07D317/10—Heterocyclic compounds containing five-membered rings having two oxygen atoms as the only ring hetero atoms having the hetero atoms in positions 1 and 3 not condensed with other rings
- C07D317/14—Heterocyclic compounds containing five-membered rings having two oxygen atoms as the only ring hetero atoms having the hetero atoms in positions 1 and 3 not condensed with other rings with substituted hydrocarbon radicals attached to ring carbon atoms
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- C07D317/10—Heterocyclic compounds containing five-membered rings having two oxygen atoms as the only ring hetero atoms having the hetero atoms in positions 1 and 3 not condensed with other rings
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Abstract
本发明公开了一种环丙基甲基酮的制备方法,其包括:乙酰丙酸甲酯与乙二醇,回流反应得3‑(2‑甲基‑1,3‑二氧杂环戊烷‑2‑基)丙酸甲酯;溶于四氢呋喃中,加入氯化锌,加入硼氢化钠,加毕,回流反应得3‑(2‑甲基‑1,3‑二氧杂环戊烷‑2‑基)丙基‑1‑醇;加入无水氯化锌和盐酸混合水溶液,回流反应得5‑氯‑2‑戊酮;5‑氯‑2‑戊酮与氢氧化钠水溶液,在90~95℃条件下反应0.5h,即可得到目标产物环丙基甲基酮。本申请工艺优选乙酰丙酸甲酯为起始原料,制备环丙基甲基酮,原料易得,成本低,利于规模化工业生产,制备工艺中,各个步骤,反应条件温和,易于控制,后处理简单,有部分中间体无需精制,可直接作为下步制备的原料,极大简化了制备工艺。
Description
技术领域
本发明属于有机合成技术领域,具体涉及一种环丙基甲基酮的制备方法。
背景技术
环丙基甲基酮是一种重要的有机原料和中间体,在医药方面,主要用于抗艾滋病药依氟维仑和伊尔雷敏的合成,在农药方面主要用于杀菌剂嘧菌环胺和环唑醇的合成。
现有技术中,一方面,传统生产环丙基甲基酮的原料采用乙酰正丙醇,通过加入盐酸氯化,然后与碱进行环合反应,得到有机层环丙基甲基酮,反应方法复杂,成本较高;另一方面,分层溶液需要通过排管依次排出,由于分层溶液整体向下的流动会使得不同的溶液之间有部分混合现象,进而使得分离收集的有机层5-氯-2-戊酮的纯度较低,进而增加了蒸馏纯化的工作量和纯化成本等问题。
发明内容
本发明所要解决的技术问题是:提供一种利于规模化工业生产的环丙基甲基酮的制备方法。
为解决上述技术问题,采用的技术方案为: 一种环丙基甲基酮的制备方法,其包括:
1)将乙酰丙酸甲酯溶于甲苯中,加入对甲苯磺酸,搅拌下加入乙二醇,升温至少回流反应10 h,气相色谱监测反应完全后,加饱和碳酸氢钠溶液淬灭反应;分出有机相并以水洗涤2次,无水硫酸钠干燥,滤除干燥剂后减压浓缩,残余物为3-(2-甲基-1,3-二氧杂环戊烷-2-基)丙酸甲酯;
2)将3-(2-甲基-1,3-二氧杂环戊烷-2-基)丙酸甲酯溶于四氢呋喃中,加入氯化锌,室温下加入硼氢化钠,加毕,回流反应4 h,加水猝灭反应,继续搅拌1 h,减压浓缩回收四氢呋喃,得3-(2-甲基-1,3-二氧杂环戊烷-2-基)丙基-1-醇粗品,无需精制,直接用于下步反应;
3)将无水氯化锌和盐酸水溶液于混合均匀,将3-(2-甲基-1,3-二氧杂环戊烷-2-基)丙基-1-醇加入反应器中,回流反应3 h,冷却至室温,以二氯甲烷萃取至少3次,合并有机相并以无水硫酸钠干燥,除干燥剂后蒸出二氯甲烷,得5-氯-2-戊酮粗品;减压蒸馏得纯度>99.6Wt.%的5-氯-2-戊酮粗品;
4)5-氯-2-戊酮与氢氧化钠水溶液,在90~95℃条件下反应0.5h,即可得到目标产物环丙基甲基酮。
反应涉及到的原料有5-氯-2-戊酮和氢氧化钠,原料廉价易得,而且反应条件在,90℃时即可反应,反应条件温和,安全可靠,适合工业生产,反应收率可达到90%以上,经过提纯,气象色谱仪中检测纯度达到99.5%以上。
步骤1)中,所述的乙酰丙酸甲酯、乙二醇与对甲苯磺酸的摩尔比为:1:1.05:0.15。
步骤2)中,所述的3-(2-甲基-1,3-二氧杂环戊烷-2-基)丙酸甲酯、氯化锌、硼氢化钠的摩尔比为1:0.2:2.25。
步骤3)中,所述的无水氯化锌、盐酸、3-(2-甲基-1,3-二氧杂环戊烷-2-基)丙基-1-醇的摩尔比为1:1.5:1;所述的HCl水溶液的质量百分含量为25~28%;
步骤4)中,所述的5-氯-2-戊酮与氢氧化钠的摩尔比为1:1.5:1;所述的HCl水溶液的质量百分含量为25~28%。
步骤3)中,所述5-氯-2-戊酮粗品,减压蒸馏粗品收集:真空达到-0.1MPa,71~72℃的馏分。
上述反应方程式为:
有益效果:本申请工艺优选乙酰丙酸甲酯为起始原料,制备环丙基甲基酮,原料易得,成本低,利于规模化工业生产,制备工艺中,各个步骤,反应条件温和,易于控制,后处理简单,有部分中间体无需精制,可直接作为下步制备的原料,极大简化了制备工艺。
具体实施方式
参照下面描述的非限制性实例,进一步描述了本发明的多层柔性管和形成方法的各个方面。
实施例1
一种环丙基甲基酮的制备方法,其包括:
1)将乙酰丙酸甲酯溶于甲苯中,加入对甲苯磺酸,搅拌下加入乙二醇,升温回流反应10 h,气相色谱监测反应完全后,加饱和碳酸氢钠溶液淬灭反应;分出有机相并以水洗涤2次,无水硫酸钠干燥,滤除干燥剂后减压浓缩,残余物为3-(2-甲基-1,3-二氧杂环戊烷-2-基)丙酸甲酯;
所述的乙酰丙酸甲酯、乙二醇与对甲苯磺酸的摩尔比为:1:1.05:0.15。
2)将3-(2-甲基-1,3-二氧杂环戊烷-2-基)丙酸甲酯溶于四氢呋喃中,加入氯化锌,室温下加入硼氢化钠,加毕,回流反应4 h,加水猝灭反应,继续搅拌1 h,减压浓缩回收四氢呋喃,得3-(2-甲基-1,3-二氧杂环戊烷-2-基)丙基-1-醇粗品,无需精制,直接用于下步反应;
所述的3-(2-甲基-1,3-二氧杂环戊烷-2-基)丙酸甲酯、氯化锌、硼氢化钠的摩尔比为1:0.2:2.25。
3)将无水氯化锌和盐酸水溶液于混合均匀,将3-(2-甲基-1,3-二氧杂环戊烷-2-基)丙基-1-醇加入反应器中,回流反应3 h,冷却至室温,以二氯甲烷萃取至少3次,合并有机相并以无水硫酸钠干燥,除干燥剂后蒸出二氯甲烷,得5-氯-2-戊酮粗品;减压蒸馏得纯度>99.6Wt.%的5-氯-2-戊酮;
所述的无水氯化锌、盐酸、3-(2-甲基-1,3-二氧杂环戊烷-2-基)丙基-1-醇的摩尔比为1:1.5:1;所述的HCl水溶液的质量百分含量为25~26%;所述5-氯-2-戊酮粗品,减压蒸馏粗品收集:真空达到-0.1MPa,71~72℃的馏分。
5-氯-2-戊酮,b.p.173℃,MS: m/z:85.0653。1H NMR,σ1.87~2.01(m,2H ),2.11(s,3H),2.68 (t,2H),3.55 (t,2H)。纯度99.9%[GC:色谱柱:DB-FFAP;检测器:FID;载气:氢气,氮气,和压缩空气的混合气体,氢气压力设置为0.3MPa;柱流量:4 mL/min;进样方式:直接进样;进样量:0.5μL; 进样器的温度设置为250℃,色谱柱温度为120℃,进样口温度:230℃;柱温:起始温度120℃,维持10 min,然后以10℃/min的速度升至200℃,维持10 min。保留时间为7.725 min]。
4)5-氯-2-戊酮与氢氧化钠水溶液,在90~95℃条件下反应0.5h,即可得到目标产物环丙基甲基酮;
所述的5-氯-2-戊酮与氢氧化钠的摩尔比为1:1.5:1;所述的HCl水溶液的质量百分含量为25~28%。
反应涉及到的原料有5-氯-2-戊酮和氢氧化钠,原料廉价易得,而且反应条件在90℃时即可反应,反应条件温和,安全可靠,适合工业生产,反应收率可达到97%,经过提纯,气象色谱仪中检测纯度达到99.9%。
环丙基甲基酮的H'-NMR:δ1.92 (t,4H)环丙基2个亚甲基上面的氢原子,δ2.83(m,1H)为直接与羰基相连的次甲基上面的1个氢原子的色谱峰,δ3.33(s, J=6.4Hz,3H)甲基。
实施例2
一种环丙基甲基酮的制备方法,其包括:
1)将乙酰丙酸甲酯溶于甲苯中,加入对甲苯磺酸,搅拌下加入乙二醇,升温回流反应11h,气相色谱监测反应完全后,加饱和碳酸氢钠溶液淬灭反应;分出有机相并以水洗涤2次,无水硫酸钠干燥,滤除干燥剂后减压浓缩,残余物为3-(2-甲基-1,3-二氧杂环戊烷-2-基)丙酸甲酯;
所述的乙酰丙酸甲酯、乙二醇与对甲苯磺酸的摩尔比为:1:1.05:0.15。
2)将3-(2-甲基-1,3-二氧杂环戊烷-2-基)丙酸甲酯溶于四氢呋喃中,加入氯化锌,室温下加入硼氢化钠,加毕,回流反应4 h,加水猝灭反应,继续搅拌1 h,减压浓缩回收四氢呋喃,得3-(2-甲基-1,3-二氧杂环戊烷-2-基)丙基-1-醇粗品,无需精制,直接用于下步反应;
所述的3-(2-甲基-1,3-二氧杂环戊烷-2-基)丙酸甲酯、氯化锌、硼氢化钠的摩尔比为1:0.2:2.25。
3)将无水氯化锌和盐酸水溶液于混合均匀,将3-(2-甲基-1,3-二氧杂环戊烷-2-基)丙基-1-醇加入反应器中,回流反应3 h,冷却至室温,以二氯甲烷萃取至少3次,合并有机相并以无水硫酸钠干燥,除干燥剂后蒸出二氯甲烷,得5-氯-2-戊酮粗品;减压蒸馏得纯度>99.6Wt.%的5-氯-2-戊酮;
所述的无水氯化锌、盐酸、3-(2-甲基-1,3-二氧杂环戊烷-2-基)丙基-1-醇的摩尔比为1:1.5:1;所述的HCl水溶液的质量百分含量为26~28%;所述5-氯-2-戊酮粗品,减压蒸馏粗品收集:真空达到-0.1MPa,71~72℃的馏分。
5-氯-2-戊酮,b.p.173℃,MS: m/z:85.0653。1H NMR,σ1.86~2.01(m,2H ),2.12(s,3H),2.69 (t,2H),3.54 (t,2H)。纯度99.8%[GC:色谱柱:DB-FFAP;检测器:FID;载气:氢气,氮气,和压缩空气的混合气体,氢气压力设置为0.3MPa;柱流量:4 mL/min;进样方式:直接进样;进样量:0.5μL; 进样器的温度设置为250℃,色谱柱温度为120℃,进样口温度:230℃;柱温:起始温度120℃,维持10 min,然后以10℃/min的速度升至200℃,维持10 min。保留时间为7.725 min]。
4)5-氯-2-戊酮与氢氧化钠水溶液,在90~95℃条件下反应0.5h,即可得到目标产物环丙基甲基酮;
所述的5-氯-2-戊酮与氢氧化钠的摩尔比为1:1.5:1;所述的HCl水溶液的质量百分含量为27~28%。
反应涉及到的原料有5-氯-2-戊酮和氢氧化钠,原料廉价易得,而且反应条件在90℃时即可反应,反应条件温和,安全可靠,适合工业生产,反应收率可达到96%,经过提纯,气象色谱仪中检测纯度达到99.8%。
环丙基甲基酮的H'-NMR:δ1.92 (t,4H)环丙基2个亚甲基上面的氢原子,δ2.83(m,1H)为直接与羰基相连的次甲基上面的1个氢原子的色谱峰,δ3.33(s, J=6.4Hz,3H)甲基。
实施例3
一种环丙基甲基酮的制备方法,其包括:
1)将乙酰丙酸甲酯溶于甲苯中,加入对甲苯磺酸,搅拌下加入乙二醇,升温至少回流反应10 h,气相色谱监测反应完全后,加饱和碳酸氢钠溶液淬灭反应;分出有机相并以水洗涤2次,无水硫酸钠干燥,滤除干燥剂后减压浓缩,残余物为3-(2-甲基-1,3-二氧杂环戊烷-2-基)丙酸甲酯;
所述的乙酰丙酸甲酯、乙二醇与对甲苯磺酸的摩尔比为:1:1.05:0.15。
2)将3-(2-甲基-1,3-二氧杂环戊烷-2-基)丙酸甲酯溶于四氢呋喃中,加入氯化锌,室温下加入硼氢化钠,加毕,回流反应4 h,加水猝灭反应,继续搅拌1 h,减压浓缩回收四氢呋喃,得3-(2-甲基-1,3-二氧杂环戊烷-2-基)丙基-1-醇粗品,无需精制,直接用于下步反应;
所述的3-(2-甲基-1,3-二氧杂环戊烷-2-基)丙酸甲酯、氯化锌、硼氢化钠的摩尔比为1:0.2:2.25。
3)将无水氯化锌和盐酸水溶液于混合均匀,将3-(2-甲基-1,3-二氧杂环戊烷-2-基)丙基-1-醇加入反应器中,回流反应3 h,冷却至室温,以二氯甲烷萃取至少3次,合并有机相并以无水硫酸钠干燥,除干燥剂后蒸出二氯甲烷,得5-氯-2-戊酮粗品;减压蒸馏得纯度>99.8Wt.%的5-氯-2-戊酮;
所述的无水氯化锌、盐酸、3-(2-甲基-1,3-二氧杂环戊烷-2-基)丙基-1-醇的摩尔比为1:1.5:1;所述的HCl水溶液的质量百分含量为25~28%;所述5-氯-2-戊酮粗品,减压蒸馏粗品收集:真空达到-0.1MPa,71~72℃的馏分。
5-氯-2-戊酮,b.p.173℃,MS: m/z:85.0653。1H NMR,σ1.88~2.02(m,2H),2.13(s,3H),2.69 (t,2H),3.56 (t,2H)。纯度99.9%[GC:色谱柱:DB-FFAP;检测器:FID;载气:氢气,氮气,和压缩空气的混合气体,氢气压力设置为0.3MPa;柱流量:4 mL/min;进样方式:直接进样;进样量:0.5μL; 进样器的温度设置为250℃,色谱柱温度为120℃,进样口温度:230℃;柱温:起始温度120℃,维持10 min,然后以10℃/min的速度升至200℃,维持10 min。保留时间为7.725 min]。
4)5-氯-2-戊酮与氢氧化钠水溶液,在90~95℃条件下反应0.5h,即可得到目标产物环丙基甲基酮;
所述的5-氯-2-戊酮与氢氧化钠的摩尔比为1:1.5:1;所述的HCl水溶液的质量百分含量为26~28%。
反应涉及到的原料有5-氯-2-戊酮和氢氧化钠,原料廉价易得,而且反应条件在90℃时即可反应,反应条件温和,安全可靠,适合工业生产,反应收率可达到95%,经过提纯,气象色谱仪中检测纯度达到99.8%。
环丙基甲基酮的H'-NMR:δ1.93 (t,4H)环丙基2个亚甲基上面的氢原子,δ2.84(m,1H)为直接与羰基相连的次甲基上面的1个氢原子的色谱峰,δ3.32(s, J=6.4Hz,3H)甲基。
Claims (6)
1.一种环丙基甲基酮的制备方法,其包括:
1)将乙酰丙酸甲酯溶于甲苯中,加入对甲苯磺酸,搅拌下加入乙二醇,升温至少回流反应10 h,气相色谱监测反应完全后,加饱和碳酸氢钠溶液淬灭反应;分出有机相并以水洗涤2次,无水硫酸钠干燥,滤除干燥剂后减压浓缩,残余物为3-(2-甲基-1,3-二氧杂环戊烷-2-基)丙酸甲酯;
2)将3-(2-甲基-1,3-二氧杂环戊烷-2-基)丙酸甲酯溶于四氢呋喃中,加入氯化锌,室温下加入硼氢化钠,加毕,回流反应2~3 h,加水猝灭反应,继续搅拌0.5 h,减压浓缩回收四氢呋喃,得3-(2-甲基-1,3-二氧杂环戊烷-2-基)丙基-1-醇粗品;
3)将无水氯化锌和盐酸水溶液混合均匀,将3-(2-甲基-1,3-二氧杂环戊烷-2-基)丙基-1-醇加入反应器中,回流反应至少2h,冷却至20~25℃,以二氯甲烷萃取至少3次,合并有机相并以无水硫酸钠干燥,除干燥剂后蒸出二氯甲烷,得5-氯-2-戊酮粗品;减压蒸馏得纯度>99.6Wt.%的5-氯-2-戊酮;
4)5-氯-2-戊酮与氢氧化钠水溶液,在90~95℃条件下反应0.5h,即可得到目标产物环丙基甲基酮。
2.根据权利要求1所述的一种环丙基甲基酮的制备方法,其特征在于:步骤1)中,所述的乙酰丙酸甲酯、乙二醇与对甲苯磺酸的摩尔比为:1:1.05:0.15。
3.根据权利要求1所述的一种环丙基甲基酮的制备方法,其特征在于:步骤2)中,所述的3-(2-甲基-1,3-二氧杂环戊烷-2-基)丙酸甲酯、氯化锌、硼氢化钠的摩尔比为1:0.2:2.25。
4.根据权利要求1所述的一种环丙基甲基酮的制备方法,其特征在于:步骤3)中,所述的无水氯化锌、盐酸、3-(2-甲基-1,3-二氧杂环戊烷-2-基)丙基-1-醇的摩尔比为1:1.5:1;所述的HCl水溶液的质量百分含量为25~28%。
5.根据权利要求1所述的一种环丙基甲基酮的制备方法,其特征在于:步骤4)中,所述的5-氯-2-戊酮与氢氧化钠的摩尔比为1:1.5:1;所述的HCl水溶液的质量百分含量为25~28%。
6.根据权利要求1所述的一种环丙基甲基酮的制备方法,其特征在于:步骤3)中,所述5-氯-2-戊酮粗品,减压蒸馏粗品收集:真空达到-0.1MPa,71~72℃的馏分。
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