SU630257A1 - Method of obtaining oxides of dialkyl (3-chlormethyl-4-methoxyaryl) phosphines - Google Patents
Method of obtaining oxides of dialkyl (3-chlormethyl-4-methoxyaryl) phosphinesInfo
- Publication number
- SU630257A1 SU630257A1 SU762378716A SU2378716A SU630257A1 SU 630257 A1 SU630257 A1 SU 630257A1 SU 762378716 A SU762378716 A SU 762378716A SU 2378716 A SU2378716 A SU 2378716A SU 630257 A1 SU630257 A1 SU 630257A1
- Authority
- SU
- USSR - Soviet Union
- Prior art keywords
- phosphines
- dialkyl
- methoxyaryl
- chlormethyl
- ppm
- Prior art date
Links
Description
33
В спектре ПМР (60 МГц, ССЦ, ГДЩС) имеетс квинтет при б 1,22 м. д. (СНз), мультиплст f 2,08 м. д. (СНг), сннглет б 4/15 м. д. (СНзО), синтлет б 4,86 м. д. (ClCHa), мультиплет б 7,66 м. д. (CgHs). Соотпоишипе иптсгралЕгИЫх нитепсивностей подтверждает правильиоеть отнесени сигпалов .In the PMR spectrum (60 MHz, SSC, GDSS) there is a quintet with b 1.22 ppm (SN3), multiplex f 2.08 ppm (SNg), bn 4/15 ppm (SNCO ), syntlet b 4.86 ppm (ClCHa), multiplet b 7.66 ppm (CgHs). Correspondingly, the use of graphed filaments confirms the correctness of the sigal assignment.
Пример 2. Окись дп-н-пропил(3-хлорметил-4-мстокепфепил )фосф1П1а.Example 2. Oxide, dp-n-propyl (3-chloromethyl-4-mstokoepfepyl) phosph1P1a.
Смесь 8 г (0,033 моль) ди-н-пропил-4метоксифеиилфосфипоксида , 35 мл копцсптрироваииой сол пой кислоты, 0,5 мл коицептрироваипой серпой кислоты и 8,5 г (0,11 моль) метилал перемешивают и нагревают при 80-90°С, пропуска при этом в реакциоппую смесь хлористый водород, к течепие 4 ч. После охлаждени и пейтрализапин реакциоппой смеси продукт выдел ют экетракпией хлороформом с последуюН1 ,ей перегонкой в вакууме. Получают 6,8 гA mixture of 8 g (0.033 mol) of di-n-propyl-4methoxypheylphosphiphoxide, 35 ml of coptic acid salt, 0.5 ml of co-acidic sickle acid and 8.5 g (0.11 mol) of methylal is stirred and heated at 80-90 ° C by passing the hydrogen chloride into the reaction mixture, for 4 hours. After cooling and the neutralized solution of the mixture, the product was isolated with ecetraction with chloroform followed by HН, by distillation in vacuum. Get 6.8 g
(70%) нелевого продукта е т. кип. 176 178°С/0,2 мм рт. ст., т. пл. перегнаппого продукта 42--44°С.(70%) of non-product e. Kip. 176 178 ° C / 0.2 mmHg Art., t. pl. distillation product 42--44 ° C.
Найдепо, %: С1 11,97; Р 10,33. СнНггСЬР.Found%: C1 11.97; R 10.33. SNNGSYR.
Вычислено, %: С1 12,29; Р 10,71.Calculated,%: C1 12.29; R 10.71.
Ф о Р м у л а изобретени Ph o Pm lu inventions
Способ получени окисей диалкнл(3хлорметнл - 4-метокеиарпл)фосфинов, заключающийс в том, что окиси диалкил(4метоксиарил )фосфина подвергают взаимодействию с параформом нли метилалем и хлористым водородом в среде копцентрчрованпой сол ной кислоты или в конпентрированпой сол ной кислоте с добавкой серной кислоты при 70-90°С.A process for producing oxides dialknl (3hlormetnl - 4-metokeiarpl) phosphines, comprising that the dialkyl oxide (4metoksiaril) phosphine is reacted with paraformaldehyde NLI methylal and hydrogen chloride in the medium koptsentrchrovanpoy hydrochloric acid or konpentrirovanpoy hydrochloric acid with addition of sulfuric acid at a 70-90 ° C.
Источники информации, прин тые во внимание при эксиертизе 1. Физер Л. и Физер М. Органическа хими , М., «Хими , т. 2, 1970, с. 327.Sources of information taken into account when examining 1. Fizer L. and Fizer M. Organic Chemistry, M., Chem., Vol. 2, 1970, p. 327.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| SU762378716A SU630257A1 (en) | 1976-07-01 | 1976-07-01 | Method of obtaining oxides of dialkyl (3-chlormethyl-4-methoxyaryl) phosphines |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| SU762378716A SU630257A1 (en) | 1976-07-01 | 1976-07-01 | Method of obtaining oxides of dialkyl (3-chlormethyl-4-methoxyaryl) phosphines |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| SU630257A1 true SU630257A1 (en) | 1978-10-30 |
Family
ID=20667908
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| SU762378716A SU630257A1 (en) | 1976-07-01 | 1976-07-01 | Method of obtaining oxides of dialkyl (3-chlormethyl-4-methoxyaryl) phosphines |
Country Status (1)
| Country | Link |
|---|---|
| SU (1) | SU630257A1 (en) |
-
1976
- 1976-07-01 SU SU762378716A patent/SU630257A1/en active
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