IES86972B2 - Pharmaceutical raw materials hexafluoroacetone synthesis method - Google Patents
Pharmaceutical raw materials hexafluoroacetone synthesis method Download PDFInfo
- Publication number
- IES86972B2 IES86972B2 IES20180078A IES20180078A IES86972B2 IE S86972 B2 IES86972 B2 IE S86972B2 IE S20180078 A IES20180078 A IE S20180078A IE S20180078 A IES20180078 A IE S20180078A IE S86972 B2 IES86972 B2 IE S86972B2
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- Ireland
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- hexafluoroacetone
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- raw materials
- mass fraction
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C45/00—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds
- C07C45/51—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by pyrolysis, rearrangement or decomposition
- C07C45/511—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by pyrolysis, rearrangement or decomposition involving transformation of singly bound oxygen functional groups to >C = O groups
- C07C45/512—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by pyrolysis, rearrangement or decomposition involving transformation of singly bound oxygen functional groups to >C = O groups the singly bound functional group being a free hydroxyl group
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
Pharmaceutical raw materials hexafluoroacetone synthesis method, comprises the following steps: 3 mol 2,3-dihydroxy-hexafluoroisopentane and 4-6 mol N-methylpropionamide were added to the reaction vessel, raised the temperature of the solution to 70-80°C for 60-80 min, then added 2-3 mol bismuth molybdate, continued to react for 50-70 min, reduced the temperature to 40-50°C, vacuum distillation, collected the fractions of 80-89°C, washed with m-cresol solution, washed with m-chloroaniline solution, recrystallized in the methoxy toluene solution, and got the finished product hexafluoroacetone.
Description
FIELD OF THE INVENTION
The present invention relates to pharmaceutical raw materials hexafluoroacetone synthesis method.
GENERAL BACKGROUND
Hexafluoroacetone is mainly used as organic solvent, copolymerization with cyclopentane can generates high temperature, conosion-resistant coatings and adhesives, synthetic medicine, it is also the raw materials pesticides, polymer materials and organic chemicals. However, most of the existing synthetic methods are using perfluoroisobutylene and potassium permanganate as the reactant, it is complicated and the final yield is not very high. Therefore, it is necessary to propose anew synthetic method for further improving the quality and yield of the product and reducing the byproduct content, it has important economic significance.
SUMMARY
The purpose of the present invention is to provide pharmaceutical raw materials hexafluoroacetone synthesis method, comprises the following steps:
(i) 3 mol 2,3-dihydroxy-hexafluoroisopentane and 4-6 mol
N-methylpropionamide were added to the reaction vessel, raisef the temperature of the solution to 70-80 C for 60-80 min, then added 2-3 mol bismuth molybdate, continued to react for 50-70 min, reduced the temperature to 40-50 °C, vacuum distillation, collected the fractions of 80-89 °C, washed with m-cresol solution, washed with m-chloroaniline solution, recrystallized in the methoxy toluene solution, got the finished product hexafluoroacetone; wherein, the mass fraction of the N-methylpropionamide solution in step (i) is 60-68%, and the vacuum distillation described in step (i) has a pressure of 10 to 20 kPa, the mass fraction of m-cresol solution in step (i) is 70 to 76%, the mass fraction of m-chloroaniline solution in step (i) is 80 to 85%, the mass fraction of methoxy toluene solution in step (i) is 92-96%.
Throughout the reaction process can be the following reaction formula:
HO^ ^CK3
ΟΗ
C4H9N + Bi2MoO6 ———► (CF352C-O.3H2O cf3
Advantage of the present invention is that: reducing intermediate links reaction, decreasing the reaction time and improving the reaction yield.
DETAILED DESCRIPTION OFPREFERRED EMBODIMENTS
The following examples with reference to specific embodiments of the present invention are further illustrated:
pharmaceutical raw materials hexafluoroacetone synthesis method.
Embodiment 1 mol 2,3-dihydroxy-hexafluoroisopentane and 4 mol N-methylpropionamide with a mass fraction of 60% were added to the reaction vessel, raised the temperature of the solution to 70 “C for 60 min, then added 2 mol bismuth molybdate, continued to react for 50 min, reduced the temperature to 40 °C, vacuum distillation at 10 kPa, collected the fractions of 80 °C, washed with m-cresol solution with a mass fraction of 70%, washed with m-chloroaniline solution with a mass fraction of 80%, recrystallized in the methoxy toluene solution with a mass fraction of 92%, got the finished product hexafluoroacetone 478.08g, yield of 96%.
Embodiment 2 mol 2,3-dihydroxy-hexafluoroisopentane and 5 mol N-methylpropionamide with a mass fraction of 65% were added to the reaction vessel, raised the temperature of the solution to 75 °C for 70 min, then added 2.5 mol bismuth molybdate, continued to react for 60 min, reduced the temperature to 45 °C, vacuum distillation at 15 kPa, collected the fractions of 85 “C, washed with m-cresol solution with a mass fraction of
Vi
73%, washed with m-chloroaniline solution with amass fraction of 82%, recrystallized in the methoxy' toluene solution with a mass fraction of 93%, got the finished product hexafluoroacetone 483.06g, yield of 97%.
Embodiment 3 mol 2,3-dihydroxy-hexafluoroisopentane and 6 mol N-methylpropionamide with a mass fraction of 68% were added to the reaction vessel, raised the temperature of the solution to 80 C for 80 min, then added 3 mol bismuth molybdate, continued to react for 70 min, reduced the temperature to 50 °C, vacuum distillation at 20 kPa, 10 collected the fractions of 89 °C, washed with m-cresol solution with a mass fraction of 76%, washed with m-chloroaniline solution with amass fraction of 85%, recrystallized in the methoxy toluene solution with a mass fraction of 96%, got the finished product hexafluoroacetone 490.53g, yield of 98.5%.
Claims (3)
1. Pharmaceutical raw materials hexafluoroacetone synthesis method, comprises the following steps: (i) 3 mol
2. ,3-dihydroxy-hexafluoroisopentane and 4-6 mol 5 N-methylpropionamide were added to the reaction vessel, raisef the temperature of the solution to 70-80 °C for 60-80 min, then added 2-3 mol bismuth molybdate, continued to react for 50-70 min, reduced the temperature to 40-50 °C, vacuum distillation, collected the fractions of 80-89 °C, washed with m-cresol solution, washed with m-chloroaniline solution, recrystallized in the methoxy toluene solution, 10 got the finished product hexafluoroacetone; wherein, the mass fraction of the N-methylpropionamide solution in step (i) is 60-68%, and the vacuum distillation described in step (i) has a pressure of 10 to 20 kPa, the mass fraction of m-cresol solution in step (i) is 70 to 76%. 15 2. Pharmaceutical raw materials hexafluoroacetone synthesis method according to claim 1 wherein the mass fraction of m-chloroaniline solution in step (1) is 80 to 85%.
3. Pharmaceutical raw materials hexafluoroacetone synthesis method according 20 to claim 1 wherein the mass fraction of methoxy toluene solution in step (i) is 92-96%.
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710215443.6A CN108238870A (en) | 2017-04-05 | 2017-04-05 | A kind of synthetic method of medical material Hexafluoro acetone |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| IES20180078A2 IES20180078A2 (en) | 2019-04-03 |
| IES86972B2 true IES86972B2 (en) | 2019-05-01 |
Family
ID=58744602
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| IES20180078A IES86972B2 (en) | 2017-04-05 | 2018-03-27 | Pharmaceutical raw materials hexafluoroacetone synthesis method |
Country Status (4)
| Country | Link |
|---|---|
| CN (1) | CN108238870A (en) |
| AU (1) | AU2018100416A4 (en) |
| GB (1) | GB201705850D0 (en) |
| IE (1) | IES86972B2 (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113527975A (en) * | 2021-07-28 | 2021-10-22 | 上海涂固安高科技有限公司 | Water-based fluorine-containing coating and preparation method thereof |
-
2017
- 2017-04-05 CN CN201710215443.6A patent/CN108238870A/en active Pending
- 2017-04-11 GB GBGB1705850.4A patent/GB201705850D0/en not_active Ceased
-
2018
- 2018-03-27 IE IES20180078A patent/IES86972B2/en unknown
- 2018-04-01 AU AU2018100416A patent/AU2018100416A4/en not_active Ceased
Also Published As
| Publication number | Publication date |
|---|---|
| GB201705850D0 (en) | 2017-05-24 |
| CN108238870A (en) | 2018-07-03 |
| IES20180078A2 (en) | 2019-04-03 |
| AU2018100416A4 (en) | 2018-05-10 |
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