CN1931864A - 高含量甲胺磷和高含量乙酰甲胺磷的制备 - Google Patents
高含量甲胺磷和高含量乙酰甲胺磷的制备 Download PDFInfo
- Publication number
- CN1931864A CN1931864A CN 200510106242 CN200510106242A CN1931864A CN 1931864 A CN1931864 A CN 1931864A CN 200510106242 CN200510106242 CN 200510106242 CN 200510106242 A CN200510106242 A CN 200510106242A CN 1931864 A CN1931864 A CN 1931864A
- Authority
- CN
- China
- Prior art keywords
- methyl
- methamidophos
- compound
- acephate
- acephatemet
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- NNKVPIKMPCQWCG-UHFFFAOYSA-N methamidophos Chemical compound COP(N)(=O)SC NNKVPIKMPCQWCG-UHFFFAOYSA-N 0.000 title claims abstract description 47
- BJWBZLUUWAJEDG-UHFFFAOYSA-N C(C)(=O)CSP(=O)(N)OC Chemical compound C(C)(=O)CSP(=O)(N)OC BJWBZLUUWAJEDG-UHFFFAOYSA-N 0.000 title abstract 3
- -1 methane halide Chemical class 0.000 claims abstract description 25
- 238000004519 manufacturing process Methods 0.000 claims abstract description 22
- 238000000034 method Methods 0.000 claims abstract description 16
- 239000002904 solvent Substances 0.000 claims abstract description 16
- YASYVMFAVPKPKE-UHFFFAOYSA-N acephate Chemical compound COP(=O)(SC)NC(C)=O YASYVMFAVPKPKE-UHFFFAOYSA-N 0.000 claims description 29
- 238000002360 preparation method Methods 0.000 claims description 19
- 239000002994 raw material Substances 0.000 claims description 11
- 150000001875 compounds Chemical class 0.000 claims description 10
- INQOMBQAUSQDDS-UHFFFAOYSA-N iodomethane Chemical compound IC INQOMBQAUSQDDS-UHFFFAOYSA-N 0.000 claims description 7
- 239000000460 chlorine Substances 0.000 claims description 6
- 229960001196 thiotepa Drugs 0.000 claims description 6
- 229910052801 chlorine Inorganic materials 0.000 claims description 5
- 230000000694 effects Effects 0.000 claims description 5
- NBVXSUQYWXRMNV-UHFFFAOYSA-N fluoromethane Chemical compound FC NBVXSUQYWXRMNV-UHFFFAOYSA-N 0.000 claims description 4
- 229910052760 oxygen Inorganic materials 0.000 claims description 4
- WQYSXVGEZYESBR-UHFFFAOYSA-N thiophosphoryl chloride Chemical compound ClP(Cl)(Cl)=S WQYSXVGEZYESBR-UHFFFAOYSA-N 0.000 claims description 4
- RDHPKYGYEGBMSE-UHFFFAOYSA-N bromoethane Chemical compound CCBr RDHPKYGYEGBMSE-UHFFFAOYSA-N 0.000 claims description 3
- 239000000126 substance Substances 0.000 claims description 3
- 230000017105 transposition Effects 0.000 claims description 3
- NEHMKBQYUWJMIP-NJFSPNSNSA-N chloro(114C)methane Chemical compound [14CH3]Cl NEHMKBQYUWJMIP-NJFSPNSNSA-N 0.000 claims description 2
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 claims 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims 1
- 239000005864 Sulphur Substances 0.000 claims 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims 1
- 239000002131 composite material Substances 0.000 claims 1
- 125000003963 dichloro group Chemical group Cl* 0.000 claims 1
- 239000001301 oxygen Substances 0.000 claims 1
- DLFVBJFMPXGRIB-UHFFFAOYSA-N Acetamide Chemical compound CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 abstract description 6
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Natural products C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 abstract 1
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 42
- 238000006243 chemical reaction Methods 0.000 description 28
- 239000000543 intermediate Substances 0.000 description 25
- PFNFFQXMRSDOHW-UHFFFAOYSA-N spermine Chemical compound NCCCNCCCCNCCCN PFNFFQXMRSDOHW-UHFFFAOYSA-N 0.000 description 16
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 15
- JZMJDSHXVKJFKW-UHFFFAOYSA-M methyl sulfate(1-) Chemical compound COS([O-])(=O)=O JZMJDSHXVKJFKW-UHFFFAOYSA-M 0.000 description 13
- 238000003756 stirring Methods 0.000 description 12
- 238000005516 engineering process Methods 0.000 description 10
- 239000007787 solid Substances 0.000 description 10
- WFDIJRYMOXRFFG-UHFFFAOYSA-N Acetic anhydride Chemical compound CC(=O)OC(C)=O WFDIJRYMOXRFFG-UHFFFAOYSA-N 0.000 description 9
- 238000009413 insulation Methods 0.000 description 8
- 229940063675 spermine Drugs 0.000 description 8
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 6
- NEHMKBQYUWJMIP-UHFFFAOYSA-N chloromethane Chemical compound ClC NEHMKBQYUWJMIP-UHFFFAOYSA-N 0.000 description 6
- WSLDOOZREJYCGB-UHFFFAOYSA-N 1,2-Dichloroethane Chemical compound ClCCCl WSLDOOZREJYCGB-UHFFFAOYSA-N 0.000 description 5
- DXJRLXNTPVIFQA-UHFFFAOYSA-N C(Cl)(Cl)Cl.C(C)(=O)N Chemical compound C(Cl)(Cl)Cl.C(C)(=O)N DXJRLXNTPVIFQA-UHFFFAOYSA-N 0.000 description 5
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 5
- 229960001701 chloroform Drugs 0.000 description 5
- 239000012535 impurity Substances 0.000 description 5
- 239000003921 oil Substances 0.000 description 5
- 239000000047 product Substances 0.000 description 5
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 4
- AXJDEHNQPMZKOS-UHFFFAOYSA-N acetylazanium;chloride Chemical class [Cl-].CC([NH3+])=O AXJDEHNQPMZKOS-UHFFFAOYSA-N 0.000 description 4
- 239000013078 crystal Substances 0.000 description 4
- 238000010792 warming Methods 0.000 description 4
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 3
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 238000005576 amination reaction Methods 0.000 description 3
- 229940050176 methyl chloride Drugs 0.000 description 3
- 239000002574 poison Substances 0.000 description 3
- 231100000614 poison Toxicity 0.000 description 3
- 238000000746 purification Methods 0.000 description 3
- 238000010992 reflux Methods 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- GZUXJHMPEANEGY-UHFFFAOYSA-N bromomethane Chemical compound BrC GZUXJHMPEANEGY-UHFFFAOYSA-N 0.000 description 2
- 239000012295 chemical reaction liquid Substances 0.000 description 2
- SUABMOWIQWUPPE-UHFFFAOYSA-N dihydrogen phosphate;methylazanium Chemical compound NC.OP(O)(O)=O SUABMOWIQWUPPE-UHFFFAOYSA-N 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000004817 gas chromatography Methods 0.000 description 2
- 239000002917 insecticide Substances 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 238000004454 trace mineral analysis Methods 0.000 description 2
- 238000004065 wastewater treatment Methods 0.000 description 2
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 1
- USFZMSVCRYTOJT-UHFFFAOYSA-N Ammonium acetate Chemical compound N.CC(O)=O USFZMSVCRYTOJT-UHFFFAOYSA-N 0.000 description 1
- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical compound [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 1
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 1
- KCPJLBUDMSTBRT-UHFFFAOYSA-N [P].ClSCl Chemical class [P].ClSCl KCPJLBUDMSTBRT-UHFFFAOYSA-N 0.000 description 1
- 125000002777 acetyl group Chemical group [H]C([H])([H])C(*)=O 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 239000003905 agrochemical Substances 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 150000003863 ammonium salts Chemical class 0.000 description 1
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 description 1
- 229910052921 ammonium sulfate Inorganic materials 0.000 description 1
- 235000011130 ammonium sulphate Nutrition 0.000 description 1
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Substances BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 description 1
- 229910052794 bromium Inorganic materials 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- VAYGXNSJCAHWJZ-UHFFFAOYSA-N dimethyl sulfate Chemical class COS(=O)(=O)OC VAYGXNSJCAHWJZ-UHFFFAOYSA-N 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000008030 elimination Effects 0.000 description 1
- 238000003379 elimination reaction Methods 0.000 description 1
- 150000002170 ethers Chemical class 0.000 description 1
- 239000012065 filter cake Substances 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 125000005843 halogen group Chemical group 0.000 description 1
- 231100000086 high toxicity Toxicity 0.000 description 1
- 229910052740 iodine Inorganic materials 0.000 description 1
- 239000011630 iodine Substances 0.000 description 1
- 229940102396 methyl bromide Drugs 0.000 description 1
- 150000005451 methyl sulfates Chemical class 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
- 239000012453 solvate Substances 0.000 description 1
- GOLXNESZZPUPJE-UHFFFAOYSA-N spiromesifen Chemical compound CC1=CC(C)=CC(C)=C1C(C(O1)=O)=C(OC(=O)CC(C)(C)C)C11CCCC1 GOLXNESZZPUPJE-UHFFFAOYSA-N 0.000 description 1
- 238000010025 steaming Methods 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
Description
Claims (4)
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN200510106242A CN1931864B (zh) | 2005-09-18 | 2005-09-18 | 高含量甲胺磷和高含量乙酰甲胺磷的制备 |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN200510106242A CN1931864B (zh) | 2005-09-18 | 2005-09-18 | 高含量甲胺磷和高含量乙酰甲胺磷的制备 |
Publications (2)
Publication Number | Publication Date |
---|---|
CN1931864A true CN1931864A (zh) | 2007-03-21 |
CN1931864B CN1931864B (zh) | 2010-05-05 |
Family
ID=37877907
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN200510106242A Expired - Fee Related CN1931864B (zh) | 2005-09-18 | 2005-09-18 | 高含量甲胺磷和高含量乙酰甲胺磷的制备 |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN1931864B (zh) |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102603795A (zh) * | 2011-01-22 | 2012-07-25 | 李坚 | 以磷酰氯为原料一步反应合成乙酰甲胺磷 |
CN104558024A (zh) * | 2014-12-28 | 2015-04-29 | 浙江大学 | 高压液相异构化生产乙酰甲胺磷的方法 |
Family Cites Families (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US5973180A (en) * | 1998-08-31 | 1999-10-26 | Bayer Corporation | Process for the production of an N-acyl derivative of O,S-dialkyl phosphoroamidothioate |
CN1133638C (zh) * | 1999-06-11 | 2004-01-07 | 湘潭大学 | 从乙酰甲胺磷原油中提取高纯度乙酰甲胺磷原粉的方法(2) |
CN1169817C (zh) * | 2002-01-28 | 2004-10-06 | 湘潭大学 | 高纯度乙酰甲胺磷原粉的制备方法(2) |
CN1176929C (zh) * | 2002-01-28 | 2004-11-24 | 湘潭大学 | 高纯度乙酰甲胺磷原粉的制备方法 |
-
2005
- 2005-09-18 CN CN200510106242A patent/CN1931864B/zh not_active Expired - Fee Related
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN102603795A (zh) * | 2011-01-22 | 2012-07-25 | 李坚 | 以磷酰氯为原料一步反应合成乙酰甲胺磷 |
CN104558024A (zh) * | 2014-12-28 | 2015-04-29 | 浙江大学 | 高压液相异构化生产乙酰甲胺磷的方法 |
CN104558024B (zh) * | 2014-12-28 | 2016-09-07 | 浙江大学 | 高压液相异构化生产乙酰甲胺磷的方法 |
Also Published As
Publication number | Publication date |
---|---|
CN1931864B (zh) | 2010-05-05 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
DE69824314T2 (de) | Derivate schiff'scher basen von ruthenium und osmium katalysatoren zur olefinmetathese | |
CN1680411A (zh) | 1,2-二氨基环己烷-铂(ⅱ)-络合物的制取方法 | |
CN102336783B (zh) | 一种异构反应 | |
WO2010086254A1 (de) | Verfahren zur herstellung von bis- und tris(silylorgano)aminen | |
CN1709897A (zh) | 化合物9,10-二氢-9-氧-10-磷杂菲的合成及其纯化工艺 | |
CN1931864A (zh) | 高含量甲胺磷和高含量乙酰甲胺磷的制备 | |
CN102775387A (zh) | 一种盐酸法舒地尔的精制方法 | |
CN101885740B (zh) | 除草剂草甘膦的制备新方法 | |
CN101619076A (zh) | 草甘膦原药的制备方法 | |
CN1931826A (zh) | 四苄基伏格列波糖的结晶及制备方法 | |
CN100408586C (zh) | 氯胺磷的制备方法 | |
CN1657531A (zh) | 草甘膦生产母液处理工艺 | |
CN1803778A (zh) | 2,4,6-三氯嘧啶的制备方法 | |
CN102603795A (zh) | 以磷酰氯为原料一步反应合成乙酰甲胺磷 | |
CN113457746B (zh) | 一种催化剂及其制备方法和应用 | |
CN101638419A (zh) | 一种除草剂中间体双甘膦的合成方法 | |
CN101054391A (zh) | 手性(1-苯乙氨基)甲基膦酸及其制备方法 | |
CN1194959C (zh) | 阳离子单体二烷基二取代基烯丙基卤化铵的制法 | |
CN100590128C (zh) | 高含量甲胺磷的制备方法 | |
CN1163499C (zh) | 旋转对映异构双(氧化膦)化合物的外消旋化方法 | |
CN101074241A (zh) | 一种制备乙酰甲胺磷的新方法 | |
CN117229266B (zh) | 一种合成雷莫司琼外消旋体及其盐的方法 | |
CN1752001A (zh) | 硫代磷酸钠的制备方法 | |
CN1288074C (zh) | 利用亚磷酸二烷基酯副产高沸物生产亚磷酸的方法 | |
CN113583044B (zh) | 一种用于预防化疗相关性恶心呕吐的药物的制备方法 |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
C06 | Publication | ||
PB01 | Publication | ||
C10 | Entry into substantive examination | ||
SE01 | Entry into force of request for substantive examination | ||
C14 | Grant of patent or utility model | ||
GR01 | Patent grant | ||
ASS | Succession or assignment of patent right |
Owner name: JIANGSU LANFENG BIO-CHEMICAL CO., LTD. Free format text: FORMER OWNER: LI JIAN Effective date: 20101222 |
|
C41 | Transfer of patent application or patent right or utility model | ||
COR | Change of bibliographic data |
Free format text: CORRECT: ADDRESS; FROM: 430074 NO.366, ZHUODAOQUAN ROAD, WUHAN CITY, HUBEI PROVINCE TO: 221400 NO.1, SUHUA ROAD, ECONOMIC DEVELOPMENT ZONE, XINYI, JIANGSU |
|
TR01 | Transfer of patent right |
Effective date of registration: 20101222 Address after: 221400, No. 1, Su Cheng Road, Xinyi Economic Development Zone, Jiangsu Patentee after: Jiangsu Lanfeng Biochemical Co., Ltd. Address before: 430074 Hubei city of Wuhan province zhuodao road 366 Patentee before: Li Jian |
|
CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20100505 Termination date: 20140918 |
|
EXPY | Termination of patent right or utility model |