SU154253A1 - - Google Patents
Info
- Publication number
- SU154253A1 SU154253A1 SU771213A SU771213A SU154253A1 SU 154253 A1 SU154253 A1 SU 154253A1 SU 771213 A SU771213 A SU 771213A SU 771213 A SU771213 A SU 771213A SU 154253 A1 SU154253 A1 SU 154253A1
- Authority
- SU
- USSR - Soviet Union
- Prior art keywords
- dehydration
- yield
- minutes
- mol
- sodium acetate
- Prior art date
Links
- 238000006297 dehydration reaction Methods 0.000 description 7
- 238000000034 method Methods 0.000 description 6
- SCVFZCLFOSHCOH-UHFFFAOYSA-M Potassium acetate Chemical compound [K+].CC([O-])=O SCVFZCLFOSHCOH-UHFFFAOYSA-M 0.000 description 5
- LGRFSURHDFAFJT-UHFFFAOYSA-N Phthalic anhydride Chemical compound C1=CC=C2C(=O)OC(=O)C2=C1 LGRFSURHDFAFJT-UHFFFAOYSA-N 0.000 description 4
- 235000011056 potassium acetate Nutrition 0.000 description 3
- VMHLLURERBWHNL-UHFFFAOYSA-M sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 description 3
- 239000001632 sodium acetate Substances 0.000 description 3
- 235000017281 sodium acetate Nutrition 0.000 description 3
- 206010057190 Respiratory tract infection Diseases 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000004821 distillation Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- -1 nitro olefins Chemical class 0.000 description 1
- 235000011091 sodium acetates Nutrition 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Description
Известен способ получени нитроолефинов дегидратацией нитроспиртов фталевым ангидридом. Недостатками его вл ютс длительность процесса и невысокий выход целевых продуктов (60-70%).A known method for the preparation of nitroolefins by the dehydration of nitrosprites with phthalic anhydride. Its disadvantages are the duration of the process and the low yield of the target products (60-70%).
Предлагаемый способ позвол ет ускорить процесс в 3 раза и увеличить выход нитроолефинов до 90%- Он заключаетс в дегидратации нитроспиртов фталевым ангидридом в присутствии ацетатов кали или натри . В примерах описано получение 1-нитропропена-1 и 1-питроамилена-1 .The proposed method makes it possible to speed up the process 3 times and increase the yield of nitroolefins up to 90%. It consists in the dehydration of nitrospirit with phthalic anhydride in the presence of potassium or sodium acetate. The examples describe the preparation of 1-nitropropene-1 and 1-pitroamylene-1.
Пример 1. Получение 1-нитропропена-1Example 1. Getting 1-nitropropene-1
а)в присутствии ацетата натри .a) in the presence of sodium acetate.
В колбу помещают 29,6 г (0,2 моль) фталевого а.нгидрида, 21 г (0,2 моль) 1-нитропропанола-2 и 0,8 г (0,01 мол ) ацетата натри , нагревают на масл ной бане до 140°, эвакуируют (70 мм рт. ст.) и температуру бапи поднимают до 170-175°.29.6 g (0.2 mol) of phthalic acid anhydride, 21 g (0.2 mol) of 1-nitropropanol-2 and 0.8 g (0.01 mol) of sodium acetate are placed in a flask, heated on an oil bath. to 140 °, evacuated (70 mm of mercury.) and the temperature of the bapi is raised to 170-175 °.
В этих услови х протекает процесс дегидратации с перегонкой иитроолефина в виде азеотроппой смеси с водой при температуре 66-70°.Under these conditions, the process of dehydration proceeds with the distillation of iitroolefin as an azeotrope mixture with water at a temperature of 66-70 °.
Продукт отдел ют от водного сло п перегон ют. Получают 1-питропропен-2 с выходом 91 %, т. кип. 65,5°С/40 мм. рт. ст.The product is separated from the aqueous layer and distilled. Get 1-pitropropen-2 with the release of 91%, so Kip. 65.5 ° C / 40 mm. Hg Art.
Врем дегидратации составл ет 20 мин. Параллельные опыты дают выход нитроолефина 91 и 93%. Продолжительность процесса дегидратации 20 и 23 мин.The dehydration time is 20 minutes. Parallel experiments yield 91% and 93% nitroolefin. The duration of the dehydration process is 20 and 23 minutes.
б)в присутствии ацетата кали .b) in the presence of potassium acetate.
Опыт провод т при температуре бани 160-165° и времени дегидратации 20 мин; выход 1-;питропропена-1 составл ет 92%.The test was carried out at a bath temperature of 160-165 ° and a dehydration time of 20 minutes; yield 1-; pitropropena-1 is 92%.
№ 154253- - 2 -No. 154253- - 2 -
. i , .- . i, .-
Пример 2. Получение -нитроамилен.а-1Example 2. Getting -nitroamil.a-1
Аналогично описаниому в примере 1 из 1-нитропентанола-2 при температуре бани 160-165° и времени дегидратации 50-55 мин получают 1-нитроамилен-1 с выходом 90-93%.Similarly to the description in example 1, 1-nitroamylene-1 is obtained from 1-nitropentanol-2 at a bath temperature of 160-165 ° and a dehydration time of 50-55 minutes with a yield of 90-93%.
Предмет изобретени Subject invention
Способ получени нитроолефи ов дегидратацией «итроспиртов фталевым ангидридом, отличающийс тем, что, с целью ускорени процесса и повышени выходов целевого продукта, процесс провод т в присутствии ацетатов натри или кали .The method of obtaining nitro olefins by dehydrating < RTI ID = 0.0 > < / RTI > ITROTHEALSPIRATES WITH PHTHALIC ANhydride, characterized in that, in order to accelerate the process and increase the yields of the desired product, the process is carried out in the presence of sodium or potassium acetates.
Publications (1)
Publication Number | Publication Date |
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SU154253A1 true SU154253A1 (en) |
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4861925A (en) * | 1988-07-15 | 1989-08-29 | W. R. Grace & Co.-Conn. | Process for the preparation of nitroolefins |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4861925A (en) * | 1988-07-15 | 1989-08-29 | W. R. Grace & Co.-Conn. | Process for the preparation of nitroolefins |
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