SU193482A1 - - Google Patents
Info
- Publication number
- SU193482A1 SU193482A1 SU1066483A SU1066483A SU193482A1 SU 193482 A1 SU193482 A1 SU 193482A1 SU 1066483 A SU1066483 A SU 1066483A SU 1066483 A SU1066483 A SU 1066483A SU 193482 A1 SU193482 A1 SU 193482A1
- Authority
- SU
- USSR - Soviet Union
- Prior art keywords
- nitrobenzene
- target product
- fluorofluorene
- fluoro
- yield
- Prior art date
Links
- LQNUZADURLCDLV-UHFFFAOYSA-N Nitrobenzene Chemical compound [O-][N+](=O)C1=CC=CC=C1 LQNUZADURLCDLV-UHFFFAOYSA-N 0.000 description 7
- VSCWAEJMTAWNJL-UHFFFAOYSA-K Aluminium chloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 description 4
- WFDIJRYMOXRFFG-UHFFFAOYSA-N acetic anhydride Chemical compound CC(=O)OC(C)=O WFDIJRYMOXRFFG-UHFFFAOYSA-N 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- JEAQRUHLKAFLNO-UHFFFAOYSA-N 1-(7-fluoro-9H-fluoren-2-yl)ethanone Chemical compound FC1=CC=C2C3=CC=C(C(=O)C)C=C3CC2=C1 JEAQRUHLKAFLNO-UHFFFAOYSA-N 0.000 description 3
- SAKIZQTUUCRVJG-UHFFFAOYSA-N 2-fluoro-9H-fluorene Chemical compound C1=CC=C2C3=CC=C(F)C=C3CC2=C1 SAKIZQTUUCRVJG-UHFFFAOYSA-N 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- QGJOPFRUJISHPQ-UHFFFAOYSA-N carbon bisulphide Chemical compound S=C=S QGJOPFRUJISHPQ-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 239000002244 precipitate Substances 0.000 description 2
- 235000019738 Limestone Nutrition 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- 239000003085 diluting agent Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000000543 intermediate Substances 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 239000006028 limestone Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
Description
Изобретение относитс к области получени важных полупродуктов дл органического синтеза.The invention relates to the field of obtaining important intermediates for organic synthesis.
Известен способ получени 2-фтор-7-ацетилфлуорена , состо щий в том, что 2-фторфлуорен подвергают взаимодействию с уксусным ангидридол в присутствии хлористого алюмини и разбавител - сероуглерода при нагревании с последующим выделением целевого продукта известным способом. Выход продукта 42%.A method of producing 2-fluoro-7-acetylfluorene is known, consisting in that 2-fluorofluorene is reacted with acetic anhydridol in the presence of aluminum chloride and the diluent carbon disulfide upon heating, followed by separation of the target product in a known manner. The yield of 42%.
Предложенный снособ отличаетс от известного тем, что процесс ведут в среде органического рстворител - нитробензола, что повышает выход целевого продукта до 72%,.The proposed removal method differs from that known in that the process is carried out in an organic solvent, nitrobenzene, which increases the yield of the target product to 72%.
Пример. К раствору 22 г (0,12 моль) 2фторфлуорена в 125 мл нитробензола при перемещивании прибавл ют 32 г (0,24 моль) хлористого алюмини (безводного), смесь нагревают до 45°С и прикапывают 12 мл (12 г, 0,12 моль) уксусного ангидрида. По окончании прибавлени смесь нагревают при 45-Example. 32 g (0.24 mol) of aluminum chloride (anhydrous) is added to a solution of 22 g (0.12 mol) of 2-fluorofluorene in 125 ml of nitrobenzene, and the mixture is heated to 45 ° C and 12 ml (12 g, 0.12 g) are added dropwise. mole) of acetic anhydride. At the end of the addition, the mixture is heated at 45
50°С 4 час и оставл ют на ночь при комнатной температуре. Далее выливают смесь в 150 г льда и 12 мл концентрированной ПС1 отгои ют нитробензол с вод ным паром и декаптируют водный раствор с осадка.50 ° C for 4 hours and left overnight at room temperature. Next, the mixture is poured into 150 g of ice and 12 ml of concentrated PS1 are distilled off with nitrobenzene with steam and the aqueous solution is decapitated from the precipitate.
Сырой осадок перекристаллизоБЫвают из 270 мл этапола с активированным углем (.Зг ).The crude precipitate is recrystallized from 270 ml of ethanol with activated charcoal (.3G).
Получают 19,45 г (72%) 2-фтор-7-ацетил флуорена, т. пл. 122-125°С.19.45 g (72%) of 2-fluoro-7-acetyl fluorene are obtained, m.p. 122-125 ° C.
Предмет изобретени Subject invention
Снособ получени 2-фтор-7-ацетилфлуорена путем взаимодействи 2-фторфлуорена с уксусным ангидридом в присутствии хлористого алюмипи при пагревапии с последующим выделением целевого продукта известпым способом , отличающийс тем, что, с целью увелть чени выхода целевого продукта, процесс ведут в среде органического растворител - нитробензола.A method for the preparation of 2-fluoro-7-acetylfluorene by reacting 2-fluorofluorene with acetic anhydride in the presence of alumi chloride during pagrevapia followed by isolation of the target product by limestone method, characterized in that, in order to increase the yield of the target product, the process is carried out in organic solvent - nitrobenzene.
Publications (1)
| Publication Number | Publication Date |
|---|---|
| SU193482A1 true SU193482A1 (en) |
Family
ID=
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| JP4301951B2 (en) | Process for the preparation of 2-halogenacyl-3-amino-acrylic acid derivatives | |
| SU1697591A3 (en) | Method of acylated diketonic compounds preparation | |
| CN102627573B (en) | Synthesis method for 5-aminolevulinic acid hydrochloride | |
| SU193482A1 (en) | ||
| US4596885A (en) | Process for the preparation of phenylglyoxylic acid esters | |
| JP3663229B2 (en) | Process for producing 4-halo-2'-nitrobutyrophenone compound | |
| WO2004087640A1 (en) | Process for the manufacture of n-alkoxalyl-alaninates | |
| CN112979555A (en) | Process for synthesizing cimetidine | |
| JPH11171829A (en) | Tri-substituted benzoic acid intermediate | |
| JP4709456B2 (en) | Method for producing benzofuranone oxime | |
| SU254501A1 (en) | METHOD FOR OBTAINING CO-NITROSOPERTIFTORCARBONOBB1B-ACID | |
| JP2002255954A (en) | METHOD FOR PRODUCING 2-n-BUTYL-5-NITROBENZOFURAN | |
| JP4598917B2 (en) | Method for producing lactone | |
| SU239962A1 (en) | METHOD OF OBTAINING 4-ALKOXYPYRIMIDO- | |
| Hamilakis et al. | Acylaminoacetyl derivatives of active methylene compounds. 3. C‐Acylation Reactions via the Hippuric Acid Azlactone | |
| SU203697A1 (en) | METHOD OF OBTAINING 2-PHENYLINOAPHTHENE OR ITS DERIVATIVES | |
| SU283222A1 (en) | METHOD OF OBTAINING N-ALKYLPYRIDYL SUBSTITUTED IMIDAZOLES | |
| JPH082891B2 (en) | Process for producing α, β-unsaturated δ-lactones | |
| SU207237A1 (en) | ||
| JP4427661B2 (en) | Process for producing 2-alkylidene-4-bromoacetoacetic acid esters | |
| SU256750A1 (en) | METHOD FOR OBTAINING CHLORODESUBLISHED ARYLOXYLKYL CARBONIC ACIDS | |
| SU197559A1 (en) | METHOD OF OBTAINING SILIC ACID 1-DIMETHYLAMINO-2-IZONITROSOBUTANON-3 | |
| SU172833A1 (en) | METHOD OF OBTAINING 2-PHENYL-3-CHLORATIONAFTENA | |
| SU358307A1 (en) | METHOD OF OBTAINING 1-METHYL-3-PHENYLCYCLOPENTANE | |
| SU278684A1 (en) | METHOD OF OBTAINING N-A1I, HJIAMHAA ALIPHATIC OR AROMATIC SERIES |