SU611591A3 - Method of obtaining stable polymorphic form of 1-oxy-3-(1',1'-dimethylheptyl)-6,6-dimethyl-6,6a,7,8,10,10a-hexahydro-9n-dibenzo-(b,d)pyrano-9-ne - Google Patents
Method of obtaining stable polymorphic form of 1-oxy-3-(1',1'-dimethylheptyl)-6,6-dimethyl-6,6a,7,8,10,10a-hexahydro-9n-dibenzo-(b,d)pyrano-9-neInfo
- Publication number
- SU611591A3 SU611591A3 SU742069769A SU2069769A SU611591A3 SU 611591 A3 SU611591 A3 SU 611591A3 SU 742069769 A SU742069769 A SU 742069769A SU 2069769 A SU2069769 A SU 2069769A SU 611591 A3 SU611591 A3 SU 611591A3
- Authority
- SU
- USSR - Soviet Union
- Prior art keywords
- dibenzo
- dimethyl
- dimethylheptyl
- hexahydro
- pyrano
- Prior art date
Links
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- -1 1, 1-dimethylheptyl Chemical group 0.000 description 1
- IXPNQXFRVYWDDI-UHFFFAOYSA-N 1-methyl-2,4-dioxo-1,3-diazinane-5-carboximidamide Chemical compound CN1CC(C(N)=N)C(=O)NC1=O IXPNQXFRVYWDDI-UHFFFAOYSA-N 0.000 description 1
- 241000220479 Acacia Species 0.000 description 1
- 229920002307 Dextran Polymers 0.000 description 1
- 108010010803 Gelatin Proteins 0.000 description 1
- 235000010643 Leucaena leucocephala Nutrition 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 229920000159 gelatin Polymers 0.000 description 1
- 239000008273 gelatin Substances 0.000 description 1
- 235000019322 gelatine Nutrition 0.000 description 1
- 235000011852 gelatine desserts Nutrition 0.000 description 1
- 229920000609 methyl cellulose Polymers 0.000 description 1
- 239000001923 methylcellulose Substances 0.000 description 1
- 235000010981 methylcellulose Nutrition 0.000 description 1
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 description 1
- 239000001267 polyvinylpyrrolidone Substances 0.000 description 1
- 229920000036 polyvinylpyrrolidone Polymers 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000001953 recrystallisation Methods 0.000 description 1
- 235000010413 sodium alginate Nutrition 0.000 description 1
- 239000000661 sodium alginate Substances 0.000 description 1
- 229940005550 sodium alginate Drugs 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
Classifications
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K31/00—Medicinal preparations containing organic active ingredients
- A61K31/33—Heterocyclic compounds
- A61K31/335—Heterocyclic compounds having oxygen as the only ring hetero atom, e.g. fungichromin
- A61K31/35—Heterocyclic compounds having oxygen as the only ring hetero atom, e.g. fungichromin having six-membered rings with one oxygen as the only ring hetero atom
- A61K31/352—Heterocyclic compounds having oxygen as the only ring hetero atom, e.g. fungichromin having six-membered rings with one oxygen as the only ring hetero atom condensed with carbocyclic rings, e.g. methantheline
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D311/00—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings
- C07D311/02—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings ortho- or peri-condensed with carbocyclic rings or ring systems
- C07D311/78—Ring systems having three or more relevant rings
- C07D311/80—Dibenzopyrans; Hydrogenated dibenzopyrans
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Pharmacology & Pharmacy (AREA)
- Epidemiology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Animal Behavior & Ethology (AREA)
- Medicinal Chemistry (AREA)
- Public Health (AREA)
- Veterinary Medicine (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
- Pyrane Compounds (AREA)
- Saccharide Compounds (AREA)
- Peptides Or Proteins (AREA)
- Medicinal Preparation (AREA)
Description
Дл предотвращени трансформации новой полиморфной формы в обычную кристаллическую форму, получаемую при перекристаллизации 1-окси -3- (, 1-димегилгептил) -6,6-димeтил-6,6a,7,8,10,10a-reкcaгидpo-9H-дибeнзo- (Ь, d)-nHpaH-9-OHa из ацетона или гексана, можно примен ть вещества, задерживающие рост кристаллов, например поливинилпирролидон , метилцеллюлозу, альгинат натри , декстран, желатин или акацию, добавл их в воду перед добавлением в нее этанольного раствора.To prevent the transformation of a new polymorphic form into the usual crystalline form, obtained by recrystallization of 1-hydroxy-3- (, 1-dimethylheptyl) -6,6-dimethyl-6,6a, 7,8,10,10a-rec-hyhydro-9H-dibenzo - (b, d) -nHpaH-9-OHa from acetone or hexane; substances that inhibit the growth of crystals, such as polyvinylpyrrolidone, methylcellulose, sodium alginate, dextran, gelatin or acacia, can be used by adding them to water before adding ethanol solution to it .
Пример. Раствор 1 г 1-окси-3-(1 1-диметилгептип ) -6,6-диметил-6,6а, 7,8,10,1 Оа-гексагидро-9Н-дибензо- (Ь, Ь)-пиран-9-она в 25 мл этанола добавл ют к 1 л воды при температуре око|ЛО 25°С при перемешивании со скоростью 300- 800 об/мин.. Перемешивание ведут около 4 час после окончани добавлен 1 этанольного раствора. Выпадает осадок 1-окси-3-(1, 1диметилгептил)-6,6-диметил-6 ,6а,7,8,9,10,10а-гексагидро-9Н-дибензо-(Ь, d)-nHpaH-9-oHa, который собирают фильтрованием.Example. A solution of 1 g of 1-hydroxy-3- (1 1-dimethylheptyp) -6,6-dimethyl-6,6a, 7,8,10,1 Oa-hexahydro-9H-dibenzo- (b, b) -pyran-9 - in 25 ml of ethanol is added to 1 l of water at an eye temperature of 25 ° C with stirring at a speed of 300-800 rpm. Stirring is carried out for about 4 hours after the end 1 ethanolic solution is added. 1-hydroxy-3- (1, 1-dimethylheptyl) -6,6-dimethyl-6, 6a, 7.8,9,10,10a-hexahydro-9H-dibenzo- (b, d) -nHpaH-9- precipitate. oHa, which is collected by filtration.
Вьшавший дибензопиранон имеет полиморфную форму с -указанными выше свойствами. Полученна микрокристаллическа форма имеет размер частиц 2,2-26 мкм, причем 50% (по объему) частиц менее 7,2 мкм.Inserted dibenzopyranone has a polymorphic form with the above properties. The resulting microcrystalline form has a particle size of 2.2-26 µm, with 50% (by volume) of particles less than 7.2 µm.
Claims (1)
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US41301173A | 1973-11-05 | 1973-11-05 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| SU611591A3 true SU611591A3 (en) | 1978-06-15 |
Family
ID=23635422
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| SU742069769A SU611591A3 (en) | 1973-11-05 | 1974-10-17 | Method of obtaining stable polymorphic form of 1-oxy-3-(1',1'-dimethylheptyl)-6,6-dimethyl-6,6a,7,8,10,10a-hexahydro-9n-dibenzo-(b,d)pyrano-9-ne |
Country Status (24)
| Country | Link |
|---|---|
| JP (1) | JPS5943463B2 (en) |
| AR (1) | AR202670A1 (en) |
| AT (1) | AT335453B (en) |
| BE (1) | BE821720A (en) |
| BG (1) | BG27088A3 (en) |
| CA (1) | CA1028715A (en) |
| CS (1) | CS174793B2 (en) |
| DD (1) | DD115660A5 (en) |
| DE (1) | DE2449927C2 (en) |
| DK (1) | DK136720B (en) |
| ES (1) | ES431672A1 (en) |
| FR (1) | FR2249665B1 (en) |
| GB (1) | GB1487635A (en) |
| HU (1) | HU167751B (en) |
| IE (1) | IE39678B1 (en) |
| IL (1) | IL45742A (en) |
| NL (1) | NL7412682A (en) |
| PH (1) | PH11719A (en) |
| PL (1) | PL94119B1 (en) |
| RO (1) | RO71769A (en) |
| SE (1) | SE407062B (en) |
| SU (1) | SU611591A3 (en) |
| YU (1) | YU287874A (en) |
| ZA (1) | ZA746029B (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4278603A (en) * | 1973-11-05 | 1981-07-14 | Eli Lilly And Company | Novel polymorphic crystalline form of dibenzopyranone |
| US4195078A (en) * | 1979-03-09 | 1980-03-25 | Eli Lilly And Company | Nabilone granulation |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3507885A (en) * | 1966-03-25 | 1970-04-21 | Hoffmann La Roche | 3-alkyl-6h-dibenzo(b,d)pyrans |
-
1974
- 1974-09-20 IE IE1949/74A patent/IE39678B1/en unknown
- 1974-09-23 ZA ZA00746029A patent/ZA746029B/en unknown
- 1974-09-25 NL NL7412682A patent/NL7412682A/en not_active Application Discontinuation
- 1974-09-27 IL IL45742A patent/IL45742A/en unknown
- 1974-09-27 PH PH16343A patent/PH11719A/en unknown
- 1974-10-01 CA CA210,510A patent/CA1028715A/en not_active Expired
- 1974-10-05 ES ES431672A patent/ES431672A1/en not_active Expired
- 1974-10-14 SE SE7412921A patent/SE407062B/en unknown
- 1974-10-17 SU SU742069769A patent/SU611591A3/en active
- 1974-10-21 DE DE2449927A patent/DE2449927C2/en not_active Expired
- 1974-10-24 AT AT856674A patent/AT335453B/en not_active IP Right Cessation
- 1974-10-28 YU YU02878/74A patent/YU287874A/en unknown
- 1974-10-31 FR FR7436368A patent/FR2249665B1/fr not_active Expired
- 1974-10-31 BE BE150088A patent/BE821720A/en not_active IP Right Cessation
- 1974-10-31 PL PL1974175276A patent/PL94119B1/pl unknown
- 1974-11-04 HU HUEI574A patent/HU167751B/hu unknown
- 1974-11-04 DK DK573374AA patent/DK136720B/en not_active IP Right Cessation
- 1974-11-04 DD DD182141A patent/DD115660A5/xx unknown
- 1974-11-04 GB GB47516/74A patent/GB1487635A/en not_active Expired
- 1974-11-04 CS CS7516A patent/CS174793B2/cs unknown
- 1974-11-05 AR AR256414A patent/AR202670A1/en active
- 1974-11-05 RO RO7480429A patent/RO71769A/en unknown
- 1974-11-05 BG BG028123A patent/BG27088A3/en unknown
- 1974-11-05 JP JP49127923A patent/JPS5943463B2/en not_active Expired
Also Published As
| Publication number | Publication date |
|---|---|
| ES431672A1 (en) | 1977-04-16 |
| HU167751B (en) | 1975-12-25 |
| AT335453B (en) | 1977-03-10 |
| GB1487635A (en) | 1977-10-05 |
| BG27088A3 (en) | 1979-08-15 |
| JPS5943463B2 (en) | 1984-10-22 |
| NL7412682A (en) | 1975-05-07 |
| DK573374A (en) | 1975-07-07 |
| BE821720A (en) | 1975-04-30 |
| PL94119B1 (en) | 1977-07-30 |
| SE7412921L (en) | 1975-05-06 |
| RO71769A (en) | 1981-09-24 |
| IL45742A (en) | 1978-06-15 |
| DD115660A5 (en) | 1975-10-12 |
| SE407062B (en) | 1979-03-12 |
| PH11719A (en) | 1978-05-30 |
| CA1028715A (en) | 1978-03-28 |
| DE2449927A1 (en) | 1975-05-07 |
| YU287874A (en) | 1984-04-30 |
| DK136720B (en) | 1977-11-14 |
| IE39678B1 (en) | 1978-12-06 |
| DK136720C (en) | 1978-04-24 |
| AU7362674A (en) | 1976-04-01 |
| IE39678L (en) | 1975-05-05 |
| CS174793B2 (en) | 1977-04-29 |
| ZA746029B (en) | 1976-04-28 |
| FR2249665A1 (en) | 1975-05-30 |
| FR2249665B1 (en) | 1978-07-21 |
| ATA856674A (en) | 1976-07-15 |
| IL45742A0 (en) | 1974-11-29 |
| JPS5082222A (en) | 1975-07-03 |
| DE2449927C2 (en) | 1985-07-04 |
| AR202670A1 (en) | 1975-06-30 |
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