SU213844A1 - METHOD OF OBTAINING DIALKYLPHOSPHONE FORMAL LIMES - Google Patents
METHOD OF OBTAINING DIALKYLPHOSPHONE FORMAL LIMESInfo
- Publication number
- SU213844A1 SU213844A1 SU1130091A SU1130091A SU213844A1 SU 213844 A1 SU213844 A1 SU 213844A1 SU 1130091 A SU1130091 A SU 1130091A SU 1130091 A SU1130091 A SU 1130091A SU 213844 A1 SU213844 A1 SU 213844A1
- Authority
- SU
- USSR - Soviet Union
- Prior art keywords
- dialkylphosphone
- limes
- formal
- obtaining
- triethylamine
- Prior art date
Links
- 239000004571 lime Substances 0.000 title 1
- ZMANZCXQSJIPKH-UHFFFAOYSA-N triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 description 10
- 238000009835 boiling Methods 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 150000001875 compounds Chemical class 0.000 description 2
- ZHNUHDYFZUAESO-UHFFFAOYSA-N formamide Chemical compound NC=O ZHNUHDYFZUAESO-UHFFFAOYSA-N 0.000 description 2
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 2
- 229910052753 mercury Inorganic materials 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 125000000217 alkyl group Chemical group 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 238000004508 fractional distillation Methods 0.000 description 1
- 150000004677 hydrates Chemical class 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 150000003017 phosphorus Chemical class 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 230000002441 reversible Effects 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Description
Изобретение касаетс получени диалкилфосфонформалкилимидов общей формулыThe invention relates to the preparation of dialkylphosphonoformalimides of the general formula
.Н О.N Oh
N-CN-C
,,
I РI P
где R, R, R - алкил.where R, R, R is alkyl.
Известен способ получени таких соединений взаимодействием диалкилхлорфоофитов с формамидом в присутствии триэтиламина.A known method for producing such compounds by reacting dialkyl chloroforites with formamide in the presence of triethylamine.
Дл повышени выхода продукта предложено названные соединени -получать взаимодействием смешанных эфироалкил-а-окси-р, р, р-трИХлорэтила,мидов кислот п тивалентного фосфора и оснований при нагревании.In order to increase the product yield, it has been proposed that the above compounds be obtained by the interaction of mixed esteralkyl-a-hydroxy-p, p, p-trichloroethyl, hydrates of hydrated phosphorus and bases upon heating.
Пример 1. В колбочку с обратным холодильником помещают 9,2 г М-пропил-Н-(а-окси-р , р, р-грихлорэтил)-амидоэтилфосфата и больщой избыток (20-25 мл) триэтиламина. Смесь нагревают при кипении триэтиламина в течение 30-40 мин. Раствор окрашиваетс в красный цо-ст. После удалени легкокип щей части в вакууме водоструйного насоса при небольшом (40 -50°С) нагревании остаток подвергают фракционной разгонке. После двух разгонок получают продукт с т. кип. 64,5- 65,5°С (2,5-10-2 лш рт. ст.); по 1,4330;Example 1. 9.2 g of M-propyl-H- (a-hydroxy-p, p, p-grhloroethyl) -amido ethyl phosphate and a large excess (20-25 ml) of triethylamine are placed in a reflux flask. The mixture is heated at the boiling point of triethylamine for 30-40 minutes. The solution is stained red. After removing the boiling part in vacuum of a water jet pump with a slight (40-50 ° C) heating, the residue is subjected to fractional distillation. After two runs, a product with m kip is obtained. 64.5- 65.5 ° С (2.5-10-2 lsh mercury); at 1.4330;
d4 1,0776. Выход 5,2 г (86, от теоретического ).d4 1.0776. Yield 5.2 g (86, from theoretical).
Найдено, %: С 42,26; 42,42; Н 8,66; 8,40; Р 13,95; 13,48; N 5,93; 6.02. MRo 53,78.Found,%: C 42.26; 42.42; H 8.66; 8.40; P 13.95; 13.48; N 5.93; 6.02. MRo 53.78.
Вычислено дл CsnisPNOi, %: С 43,05; Н 8,07; Р 13,90; N 6,29. ЛШо 53,35.Calculated for CsnisPNOi,%: C 43.05; H 8.07; P 13.90; N 6.29. LSH 53.35.
Пример 2. В колбочку с обратиым холодильником помешают 11,4 г М-этил-М-{а-оксиР ,р,р-трихлорэтил)-амидрдиэтилфосфата и избыток триэтиламина (25-30 мл). Смесь нагревают при кипении триэтиламина .около 1 час, нри этом раство,р темнеет. Летучие компоненты удал ют в вакууме, а остаток после двух перегонок дает продукт с т. кип. 59,5- 60°С (2,5-10-- лиг рт. ст.); по 1,4319;Example 2. In a flask with a reversible cooler, 11.4 g of M-ethyl-M- {a-oxyP, p, p-trichloroethyl) -amydiethylphosphate and an excess of triethylamine (25-30 ml) will be placed. The mixture is heated at the boiling point of triethylamine. About 1 hour, at this solution, p darkens. The volatile components are removed in vacuo, and the residue after two distillations yields a product with bale. 59.5-60 ° C (2.5-10-- ligus mercury); at 1.4319;
dd
1,1070. Выход 5,8 г (80,5о/о от теоретического ).1,1070. Yield 5.8 g (80.5o / o from theoretical).
Найдено, %: С 40,14; 40,24; Н 7,83; 8,02; Р 14,42; 14,64. MRo 48,96.Found,%: C 40.14; 40.24; H 7.83; 8.02; R 14.42; 14.64. MRo 48.96.
Вычислено дл СуНюРМО, . С 40,19; Н 7,66; Р 14,83. MRo 48,73.Calculated for SUNURMO,. C 40.19; H 7.66; R 14.83. MRo 48.73.
2525
Предмет изобретени 3 ламиды кислот п тивалентного фосфора подвергают взаимодействию с основани ми при нагреваний, 4 2. Способ по п. 1, отличающийс тем, что натревание ведут до температуры кипени основани .The subject of the invention 3 lamides of pivalent phosphorus acids is reacted with bases upon heating, 4 2. The method according to claim 1, wherein heating is carried out up to the boiling point of the base.
Publications (1)
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SU213844A1 true SU213844A1 (en) |
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