SU203681A1 - FURTHER RECEIVING FRIENILHYD1> & AZIDOVALIDE Phosphoric acids - Google Patents
FURTHER RECEIVING FRIENILHYD1> & AZIDOVALIDE Phosphoric acidsInfo
- Publication number
- SU203681A1 SU203681A1 SU1104399A SU1104399A SU203681A1 SU 203681 A1 SU203681 A1 SU 203681A1 SU 1104399 A SU1104399 A SU 1104399A SU 1104399 A SU1104399 A SU 1104399A SU 203681 A1 SU203681 A1 SU 203681A1
- Authority
- SU
- USSR - Soviet Union
- Prior art keywords
- azidovalide
- phosphoric acids
- further receiving
- ether
- cooling
- Prior art date
Links
- 235000011007 phosphoric acid Nutrition 0.000 title 1
- 150000003016 phosphoric acids Chemical class 0.000 title 1
- RTZKZFJDLAIYFH-UHFFFAOYSA-N diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 12
- 239000002253 acid Substances 0.000 claims description 7
- HKOOXMFOFWEVGF-UHFFFAOYSA-N Phenylhydrazine Chemical compound NNC1=CC=CC=C1 HKOOXMFOFWEVGF-UHFFFAOYSA-N 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 4
- 229940067157 phenylhydrazine Drugs 0.000 claims description 4
- 150000001805 chlorine compounds Chemical class 0.000 claims description 2
- 238000000034 method Methods 0.000 claims description 2
- 239000003960 organic solvent Substances 0.000 claims description 2
- 238000002360 preparation method Methods 0.000 claims description 2
- 150000007513 acids Chemical class 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 229940042795 Hydrazides for tuberculosis treatment Drugs 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- 230000000875 corresponding Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 238000002329 infrared spectrum Methods 0.000 description 1
- 239000000543 intermediate Substances 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 229910052573 porcelain Inorganic materials 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
Description
Насто щее изобретение касаетс способа получени фенилгидразидов диалкилфосфористых кислот общей формулы (RO)2PNHNHCeH5, которые могут найти применение в качестве полупродуктов органического синтеза.The present invention relates to a process for the preparation of phenyl hydrazides of dialkylphosphorous acids of the general formula (RO) 2PNHNHCeH5, which can be used as intermediates for organic synthesis.
Предлагаемый способ состоит в том, что хлорангидриды диалкилфосфористых кислот подвергают взаимодействию с фенилгидразином в среде органического растворител , например эфира, при охлаждении не выше 0°С.The proposed method consists in the fact that the acid chlorides of dialkylphosphorous acids are reacted with phenylhydrazine in an organic solvent medium, for example ether, upon cooling not higher than 0 ° C.
Пример. В четырехгорлую колбу, снабженную мешалкой, обратным холодильником, капельной воронкой и термометром, помещают 21,64 г (0,2 моль) фенилгидразина в 250 мл абсолютного эфира. К этой смеси при охлаждении ее до -2°С прикапывают раствор 21,25 г (0,1 моль) хлорангидрида дибутилфосфористой кислоты в 50 мл эфира. Температуру поддерживают не выше 0°С.Example. In a four-necked flask equipped with a stirrer, a reflux condenser, an addition funnel and a thermometer, 21.64 g (0.2 mol) of phenylhydrazine are placed in 250 ml of absolute ether. To this mixture, while cooling it to -2 ° C, a solution of 21.25 g (0.1 mol) of dibutylphosphorous acid chloride in 50 ml of ether is added dropwise. The temperature is maintained no higher than 0 ° C.
По окончании прикапывани смесь перемешивают еп1,е в течение 1 час, а затем осадокAt the end of the dropping, the mixture is stirred for en1, e for 1 hour, and then the precipitate
СОЛЯНОКИСЛОГО фенилгидразина отфильтровывают и промывают эфиром.SOLYANO ACID phenylhydrazine is filtered off and washed with ether.
Фильтрат выливают в фарфоровую чашку. После испарени эфира в чашке остаютс белые кристаллы, по данным элементарного анализа и ИК-спектрам, отвечающие формулеThe filtrate is poured into a porcelain cup. After evaporation of the ether, white crystals remain in the dish, according to elementary analysis and IR spectra, corresponding to the formula
..
Р--К1ПЫНСбПд.R - K1PYNSbPd.
CiHgO/CiHgO /
Выход 60-65% от теоретического. Найдено, %: Р 10,92, 11,11; N 9,64, 9,71. Вычислено, %: Р 10,92; N 9,85.Output 60-65% of theoretical. Found,%: P 10.92, 11.11; N 9.64, 9.71. Calculated,%: R 10.92; N 9.85.
Предмет изобретени Subject invention
Claims (2)
Publications (1)
| Publication Number | Publication Date |
|---|---|
| SU203681A1 true SU203681A1 (en) |
Family
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