CN102993112A - 4, 4’-二氨基二苯乙烯-2, 2’-二磺酸衍生物 - Google Patents
4, 4’-二氨基二苯乙烯-2, 2’-二磺酸衍生物 Download PDFInfo
- Publication number
- CN102993112A CN102993112A CN2012102240034A CN201210224003A CN102993112A CN 102993112 A CN102993112 A CN 102993112A CN 2012102240034 A CN2012102240034 A CN 2012102240034A CN 201210224003 A CN201210224003 A CN 201210224003A CN 102993112 A CN102993112 A CN 102993112A
- Authority
- CN
- China
- Prior art keywords
- compound
- compd
- disulfonic acid
- preparation
- alkyl
- 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
- REJHVSOVQBJEBF-OWOJBTEDSA-N 5-azaniumyl-2-[(e)-2-(4-azaniumyl-2-sulfonatophenyl)ethenyl]benzenesulfonate Chemical class OS(=O)(=O)C1=CC(N)=CC=C1\C=C\C1=CC=C(N)C=C1S(O)(=O)=O REJHVSOVQBJEBF-OWOJBTEDSA-N 0.000 title abstract 3
- 150000001875 compounds Chemical class 0.000 claims description 45
- 239000002253 acid Substances 0.000 claims description 17
- 238000004043 dyeing Methods 0.000 abstract description 15
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 abstract description 10
- 239000006081 fluorescent whitening agent Substances 0.000 abstract description 5
- 125000002887 hydroxy group Chemical group [H]O* 0.000 abstract description 5
- 125000002490 anilino group Chemical group [H]N(*)C1=C([H])C([H])=C([H])C([H])=C1[H] 0.000 abstract description 4
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 abstract description 3
- 238000005265 energy consumption Methods 0.000 abstract description 3
- 125000005843 halogen group Chemical group 0.000 abstract description 3
- 229910052739 hydrogen Inorganic materials 0.000 abstract description 3
- 239000001257 hydrogen Substances 0.000 abstract description 3
- 229910052760 oxygen Inorganic materials 0.000 abstract description 3
- 229910052717 sulfur Inorganic materials 0.000 abstract description 3
- 125000000217 alkyl group Chemical group 0.000 abstract 3
- 125000005842 heteroatom Chemical group 0.000 abstract 1
- 125000004435 hydrogen atom Chemical group [H]* 0.000 abstract 1
- 238000002360 preparation method Methods 0.000 description 27
- 238000006243 chemical reaction Methods 0.000 description 16
- 239000012043 crude product Substances 0.000 description 16
- LVTJOONKWUXEFR-FZRMHRINSA-N protoneodioscin Natural products O(C[C@@H](CC[C@]1(O)[C@H](C)[C@@H]2[C@]3(C)[C@H]([C@H]4[C@@H]([C@]5(C)C(=CC4)C[C@@H](O[C@@H]4[C@H](O[C@H]6[C@@H](O)[C@@H](O)[C@@H](O)[C@H](C)O6)[C@@H](O)[C@H](O[C@H]6[C@@H](O)[C@@H](O)[C@@H](O)[C@H](C)O6)[C@H](CO)O4)CC5)CC3)C[C@@H]2O1)C)[C@H]1[C@H](O)[C@H](O)[C@H](O)[C@@H](CO)O1 LVTJOONKWUXEFR-FZRMHRINSA-N 0.000 description 16
- 239000000243 solution Substances 0.000 description 15
- 239000000975 dye Substances 0.000 description 14
- 238000006467 substitution reaction Methods 0.000 description 13
- 229920000742 Cotton Polymers 0.000 description 12
- LWLSVNFEVKJDBZ-UHFFFAOYSA-N N-[4-(trifluoromethoxy)phenyl]-4-[[3-[5-(trifluoromethyl)pyridin-2-yl]oxyphenyl]methyl]piperidine-1-carboxamide Chemical compound FC(OC1=CC=C(C=C1)NC(=O)N1CCC(CC1)CC1=CC(=CC=C1)OC1=NC=C(C=C1)C(F)(F)F)(F)F LWLSVNFEVKJDBZ-UHFFFAOYSA-N 0.000 description 12
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 12
- OMFXVFTZEKFJBZ-HJTSIMOOSA-N corticosterone Chemical compound O=C1CC[C@]2(C)[C@H]3[C@@H](O)C[C@](C)([C@H](CC4)C(=O)CO)[C@@H]4[C@@H]3CCC2=C1 OMFXVFTZEKFJBZ-HJTSIMOOSA-N 0.000 description 10
- 238000000034 method Methods 0.000 description 10
- 238000010792 warming Methods 0.000 description 10
- 0 *C(C=CC1)=C*1=CN* Chemical compound *C(C=CC1)=C*1=CN* 0.000 description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 9
- 239000000835 fiber Substances 0.000 description 8
- 238000004128 high performance liquid chromatography Methods 0.000 description 7
- 238000012916 structural analysis Methods 0.000 description 7
- 238000005406 washing Methods 0.000 description 7
- 150000002148 esters Chemical class 0.000 description 6
- 238000001035 drying Methods 0.000 description 5
- 238000005507 spraying Methods 0.000 description 5
- 206010013786 Dry skin Diseases 0.000 description 4
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 4
- 239000007864 aqueous solution Substances 0.000 description 4
- 229910052799 carbon Inorganic materials 0.000 description 4
- MGNCLNQXLYJVJD-UHFFFAOYSA-N cyanuric chloride Chemical compound ClC1=NC(Cl)=NC(Cl)=N1 MGNCLNQXLYJVJD-UHFFFAOYSA-N 0.000 description 4
- 239000004744 fabric Substances 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 238000010992 reflux Methods 0.000 description 4
- 125000006414 CCl Chemical group ClC* 0.000 description 3
- YNAVUWVOSKDBBP-UHFFFAOYSA-N Morpholine Chemical compound C1COCCN1 YNAVUWVOSKDBBP-UHFFFAOYSA-N 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 239000012467 final product Substances 0.000 description 3
- 238000012423 maintenance Methods 0.000 description 3
- 230000005855 radiation Effects 0.000 description 3
- 239000011734 sodium Substances 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 description 2
- -1 Anilino Chemical group 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 2
- 125000003368 amide group Chemical group 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 238000009413 insulation Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 2
- 238000007639 printing Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 229920006395 saturated elastomer Polymers 0.000 description 2
- 235000017550 sodium carbonate Nutrition 0.000 description 2
- 229910000029 sodium carbonate Inorganic materials 0.000 description 2
- 229910052938 sodium sulfate Inorganic materials 0.000 description 2
- 235000011152 sodium sulphate Nutrition 0.000 description 2
- 239000004753 textile Substances 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- QLRBNEZOQPLERN-UHFFFAOYSA-N (sulfonylamino)benzene Chemical compound O=S(=O)=NC1=CC=CC=C1 QLRBNEZOQPLERN-UHFFFAOYSA-N 0.000 description 1
- MBDUIEKYVPVZJH-UHFFFAOYSA-N 1-ethylsulfonylethane Chemical class CCS(=O)(=O)CC MBDUIEKYVPVZJH-UHFFFAOYSA-N 0.000 description 1
- CDAWCLOXVUBKRW-UHFFFAOYSA-N 2-aminophenol Chemical compound NC1=CC=CC=C1O CDAWCLOXVUBKRW-UHFFFAOYSA-N 0.000 description 1
- 229940126062 Compound A Drugs 0.000 description 1
- NLDMNSXOCDLTTB-UHFFFAOYSA-N Heterophylliin A Natural products O1C2COC(=O)C3=CC(O)=C(O)C(O)=C3C3=C(O)C(O)=C(O)C=C3C(=O)OC2C(OC(=O)C=2C=C(O)C(O)=C(O)C=2)C(O)C1OC(=O)C1=CC(O)=C(O)C(O)=C1 NLDMNSXOCDLTTB-UHFFFAOYSA-N 0.000 description 1
- 235000000177 Indigofera tinctoria Nutrition 0.000 description 1
- 241000208202 Linaceae Species 0.000 description 1
- 235000004431 Linum usitatissimum Nutrition 0.000 description 1
- ZMCHBSMFKQYNKA-UHFFFAOYSA-N Nc(cccc1)c1S(O)(=O)=O Chemical compound Nc(cccc1)c1S(O)(=O)=O ZMCHBSMFKQYNKA-UHFFFAOYSA-N 0.000 description 1
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 238000010009 beating Methods 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 230000000295 complement effect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- ZBCBWPMODOFKDW-UHFFFAOYSA-N diethanolamine Chemical compound OCCNCCO ZBCBWPMODOFKDW-UHFFFAOYSA-N 0.000 description 1
- 238000010981 drying operation Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 229940097275 indigo Drugs 0.000 description 1
- COHYTHOBJLSHDF-UHFFFAOYSA-N indigo powder Natural products N1C2=CC=CC=C2C(=O)C1=C1C(=O)C2=CC=CC=C2N1 COHYTHOBJLSHDF-UHFFFAOYSA-N 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 239000001103 potassium chloride Substances 0.000 description 1
- 235000011164 potassium chloride Nutrition 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- 230000000750 progressive effect Effects 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 159000000000 sodium salts Chemical class 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000009941 weaving Methods 0.000 description 1
- 230000002087 whitening effect Effects 0.000 description 1
- 210000002268 wool Anatomy 0.000 description 1
Landscapes
- Coloring (AREA)
Abstract
Description
Claims (1)
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201210224003.4A CN102993112B (zh) | 2011-06-30 | 2012-06-29 | 4,4’-二氨基二苯乙烯-2,2’-二磺酸衍生物 |
Applications Claiming Priority (4)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201110182826.0 | 2011-06-30 | ||
CN201110182826 | 2011-06-30 | ||
CN2011101828260 | 2011-06-30 | ||
CN201210224003.4A CN102993112B (zh) | 2011-06-30 | 2012-06-29 | 4,4’-二氨基二苯乙烯-2,2’-二磺酸衍生物 |
Publications (2)
Publication Number | Publication Date |
---|---|
CN102993112A true CN102993112A (zh) | 2013-03-27 |
CN102993112B CN102993112B (zh) | 2015-04-29 |
Family
ID=47922286
Family Applications (5)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN201210224487.2A Expired - Fee Related CN102993111B (zh) | 2011-06-30 | 2012-06-29 | 4,4’-二氨基二苯乙烯-2,2’-二磺酸衍生物的制备方法 |
CN201210223973.2A Expired - Fee Related CN102993110B (zh) | 2011-06-30 | 2012-06-29 | 4,4’-二氨基二苯乙烯-2,2’-二磺酸衍生物的中间体 |
CN201210223744.0A Expired - Fee Related CN102993770B (zh) | 2011-06-30 | 2012-06-29 | 4, 4’-二氨基二苯乙烯-2, 2’-二磺酸衍生物的应用 |
CN201210224020.8A Expired - Fee Related CN102993113B (zh) | 2011-06-30 | 2012-06-29 | 4, 4’-二氨基二苯乙烯-2, 2’-二磺酸衍生物 |
CN201210224003.4A Expired - Fee Related CN102993112B (zh) | 2011-06-30 | 2012-06-29 | 4,4’-二氨基二苯乙烯-2,2’-二磺酸衍生物 |
Family Applications Before (4)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN201210224487.2A Expired - Fee Related CN102993111B (zh) | 2011-06-30 | 2012-06-29 | 4,4’-二氨基二苯乙烯-2,2’-二磺酸衍生物的制备方法 |
CN201210223973.2A Expired - Fee Related CN102993110B (zh) | 2011-06-30 | 2012-06-29 | 4,4’-二氨基二苯乙烯-2,2’-二磺酸衍生物的中间体 |
CN201210223744.0A Expired - Fee Related CN102993770B (zh) | 2011-06-30 | 2012-06-29 | 4, 4’-二氨基二苯乙烯-2, 2’-二磺酸衍生物的应用 |
CN201210224020.8A Expired - Fee Related CN102993113B (zh) | 2011-06-30 | 2012-06-29 | 4, 4’-二氨基二苯乙烯-2, 2’-二磺酸衍生物 |
Country Status (1)
Country | Link |
---|---|
CN (5) | CN102993111B (zh) |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN107245058A (zh) * | 2017-07-03 | 2017-10-13 | 上海安诺其集团股份有限公司 | 二苯乙烯型化合物、其中间体、制备方法和应用 |
Families Citing this family (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN103468017B (zh) * | 2013-09-02 | 2015-04-01 | 山西青山化工有限公司 | 一种超白高效低杂质荧光增白剂的制备方法 |
Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO1998014435A1 (en) * | 1996-10-02 | 1998-04-09 | Dystar, L., P. | Fiber-reactive brighteners of bis-s-triazinylaminostilbene |
JP2001330935A (ja) * | 2000-05-18 | 2001-11-30 | Fuji Photo Film Co Ltd | 認証性が付与されたハロゲン化銀写真要素、記録材料および認証識別方法 |
Family Cites Families (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE1469218B1 (de) * | 1964-06-30 | 1971-09-08 | Hoechst Ag | 4,4'-Bis-triazinylamino-stilbenverbindungen und ihre Verwendung als reaktive optischeAufhellungsmittel |
CH640899A5 (en) * | 1979-05-14 | 1984-01-31 | Ciba Geigy Ag | Stable stilbene brightener solutions |
US5741905A (en) * | 1994-07-23 | 1998-04-21 | Ciba Specialty Chemicals Corporation | Triazine ultraviolet absorbers useful for improving the sun protection factor of textiles |
GB9503474D0 (en) * | 1995-02-22 | 1995-04-12 | Ciba Geigy Ag | Compounds and their use |
CN101298437A (zh) * | 2008-06-27 | 2008-11-05 | 山东大学 | 含对氨基苯甲酸基团季铵盐型荧光增白剂及其合成与应用 |
-
2012
- 2012-06-29 CN CN201210224487.2A patent/CN102993111B/zh not_active Expired - Fee Related
- 2012-06-29 CN CN201210223973.2A patent/CN102993110B/zh not_active Expired - Fee Related
- 2012-06-29 CN CN201210223744.0A patent/CN102993770B/zh not_active Expired - Fee Related
- 2012-06-29 CN CN201210224020.8A patent/CN102993113B/zh not_active Expired - Fee Related
- 2012-06-29 CN CN201210224003.4A patent/CN102993112B/zh not_active Expired - Fee Related
Patent Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO1998014435A1 (en) * | 1996-10-02 | 1998-04-09 | Dystar, L., P. | Fiber-reactive brighteners of bis-s-triazinylaminostilbene |
JP2001330935A (ja) * | 2000-05-18 | 2001-11-30 | Fuji Photo Film Co Ltd | 認証性が付与されたハロゲン化銀写真要素、記録材料および認証識別方法 |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN107245058A (zh) * | 2017-07-03 | 2017-10-13 | 上海安诺其集团股份有限公司 | 二苯乙烯型化合物、其中间体、制备方法和应用 |
Also Published As
Publication number | Publication date |
---|---|
CN102993111A (zh) | 2013-03-27 |
CN102993110A (zh) | 2013-03-27 |
CN102993111B (zh) | 2015-11-25 |
CN102993110B (zh) | 2015-06-24 |
CN102993770B (zh) | 2014-06-25 |
CN102993113B (zh) | 2015-04-29 |
CN102993113A (zh) | 2013-03-27 |
CN102993112B (zh) | 2015-04-29 |
CN102993770A (zh) | 2013-03-27 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
RU2291925C2 (ru) | Способ трехцветного окрашивания или печати по материалам из синтетического полиамидного волокна и реакционноспособный краситель | |
BRPI0914939B1 (pt) | Tintas ácidas, seus usos e processo para preparação das mesmas | |
CN102993770B (zh) | 4, 4’-二氨基二苯乙烯-2, 2’-二磺酸衍生物的应用 | |
Czajkowski et al. | Synthesis of bifunctional monochlorotriazine reactive dyes increasing UV-protection properties of cotton fabrics | |
CN110387141A (zh) | 一种染料母体为苯并噻唑类的偶氮阳离子活性染料及其制备和应用 | |
CN104016880B (zh) | 专用偶氮活性分散染料的前驱体及用途 | |
CN105754376A (zh) | 一种偶合组分为n,n-二乙基间氨基苯胺的阳离子活性染料及其制备方法和应用 | |
Chen et al. | Study on coloration of silk based on coupling reaction with a diazonium compound | |
JP2009007724A (ja) | 酸性染料の染色方法。 | |
CN105733301A (zh) | 一种偶合组分为间氨基乙酰苯胺的阳离子活性染料及其制备方法和应用 | |
CN102504582B (zh) | 一种活性深蓝双偶氮染料及其制备方法 | |
CN107245058A (zh) | 二苯乙烯型化合物、其中间体、制备方法和应用 | |
JPH1129714A (ja) | アントラピリドン化合物を用いることを特徴とするポリアミド系繊維の染色法及び染色物 | |
CN109796786B (zh) | 一种复合型鲜艳红色活性染料及其制备方法与应用 | |
CN105733300A (zh) | 一种偶合组分为苯胺的阳离子活性染料及其制备方法和应用 | |
CH641197A5 (de) | Reaktive monoazofarbstoffe und verfahren zu deren herstellung. | |
Otutu et al. | Synthesis of disazo disperse dye compounds derived from 4-bromoaniline and 3-aminophenol as potential near infra-red absorbers. | |
CN104119692A (zh) | 一种活性橙染料化合物及其应用 | |
CN110128846B (zh) | 一种藏青色活性染料及其制备方法 | |
CN107325584A (zh) | 4,4’‑二氨基二苯乙烯‑2,2’‑二磺酸化合物、其中间体、制备方法和应用 | |
CN103013168A (zh) | 一种黄色双活性基染料化合物、制备方法及其组合物 | |
CN103030990A (zh) | 一种偶氮化合物的应用 | |
CN110294718B (zh) | 一种偶氮类紫红色染料母体及制备方法与应用 | |
US3152108A (en) | Iothiuronium salts of 2-haloethyl sulfide dyestuffs | |
JPH05125036A (ja) | 非対称シユウ酸ジアリールアミド |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
C06 | Publication | ||
PB01 | Publication | ||
C10 | Entry into substantive examination | ||
SE01 | Entry into force of request for substantive examination | ||
C53 | Correction of patent of invention or patent application | ||
CB02 | Change of applicant information |
Address after: Liantang Town Qingpu District Shanghai city 201717 Zhu Feng Road No. 6188 room 2622 Applicant after: SHANGHAI ANOKY GROUP CO., LTD. Address before: Liantang Town Qingpu District Shanghai city 201717 Zhu Feng Road No. 6188 room 2622 Applicant before: Shanghai ANOKY Textile Chemicals Co., Ltd. |
|
COR | Change of bibliographic data |
Free format text: CORRECT: APPLICANT; FROM: SHANGHAI ANOKY TEXTILE CHEMICALS CO., LTD. TO: SHANGHAI ANOKY GROUP CO., LTD. |
|
C14 | Grant of patent or utility model | ||
GR01 | Patent grant | ||
TR01 | Transfer of patent right | ||
TR01 | Transfer of patent right |
Effective date of registration: 20171121 Address after: 224631 Jiangsu province Yancheng City county road six North Ring Chen Zhen Wei Patentee after: JIANGSU ANOKY CHEMICAL CO., LTD. Address before: Liantang Town Qingpu District Shanghai city 201717 Zhu Feng Road No. 6188 room 2622 Patentee before: SHANGHAI ANOKY GROUP CO., LTD. |
|
TR01 | Transfer of patent right | ||
TR01 | Transfer of patent right |
Effective date of registration: 20190808 Address after: 201703 Shanghai city Qingpu District Songhua Road No. 881 Co-patentee after: Yantai Anoky Fine Chemical Co., Ltd. Patentee after: SHANGHAI ANOKY GROUP CO., LTD. Co-patentee after: SHANGHAI ANOKY DIGITAL TECHNOLOGY CO., LTD. Co-patentee after: Dongying Annuoqi Textile Material Co., Ltd. Co-patentee after: Shanghai Shangyu Digital Technology Co., Ltd. Co-patentee after: Yantai Shangyu Digital Technology Co., Ltd. Address before: 224631 North of Weiliu Road, Chenjiagang Town, Xiangshui County, Yancheng City, Jiangsu Province Patentee before: JIANGSU ANOKY CHEMICAL CO., LTD. |
|
CF01 | Termination of patent right due to non-payment of annual fee | ||
CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20150429 Termination date: 20200629 |