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SU202943A1 - METHOD OF OBTAINING ANHYDRIDES OF 5-ALKYLMETHYLTIO-PHOSPHONE ACIDS - Google Patents

METHOD OF OBTAINING ANHYDRIDES OF 5-ALKYLMETHYLTIO-PHOSPHONE ACIDS

Info

Publication number
SU202943A1
SU202943A1 SU969215A SU969215A SU202943A1 SU 202943 A1 SU202943 A1 SU 202943A1 SU 969215 A SU969215 A SU 969215A SU 969215 A SU969215 A SU 969215A SU 202943 A1 SU202943 A1 SU 202943A1
Authority
SU
USSR - Soviet Union
Prior art keywords
anhydrides
alkylmethyltio
obtaining
phosphone
acids
Prior art date
Application number
SU969215A
Other languages
Russian (ru)
Original Assignee
Б. М. Гладштейн, Б. Л. Захаров , И. А. Ачкасов
Publication of SU202943A1 publication Critical patent/SU202943A1/en

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Description

Данное изобретение относитс  к способу получени  производных кислот фосфора, которые могут быть применены в качестве инсектицидов , добавок к смазочным массам. Предложен способ получени  ангидридов S-алкилметилтиофосфоновых кислот, заключающийс  в том, что О-алкил-5-алкилметилтиофосфонаты ввод т в реакцию с бромистым ацетилом. Реакцию нровод т при 50- 60°С. Пример. Смесь 26,73 г (0,159 моль) 0-этил-5-этилметилтиофосфоната и 8,34 г (0,068 моль) бромистого ацетила нагревают до 55-60°С в течение 12 час. Легколетучие продукты удал ют, остаток перегон ют. 1 фракци : О-этил-5-этилметилтиофосфо-50°С/0 ,04 мм, п нат (14,56 г) т. кии. 1,4750. Исходный О-этил-З-этилметилтиофос 1,4750. фонат: т. кин. 65-70°С/1 II фракци : ангидрид S-этилметилтиофосфоновой кислоты (4,76 г) (54о/а от теоретического ) т. кин. 120-125°С/0,04 мм, df 1,2563, п 1,5200 MRo 63,42; вычислено: 64,22. Найдено, %: С 28,15, 28,40; Н 6,00; 6,25; Р 24,05; 24,22; S 24,28; 24,69. CeHjgOsPaSa. Вычислено, %: С 27,47; Н 6,14; Р 23,61; S 24,45. Предмет изобретени  Снособ нолучени  ангидридов S-алкилметилтнофосфоновых кислот, отличающийс  тем, что О-алкил-5-алкилметилтиофосфонаты ввод т в реакцию с бромистым ацетилом нри 50-60°С.This invention relates to a process for the preparation of phosphorus acid derivatives which can be used as insecticides, additives to lubricating masses. A method has been proposed for the preparation of S-alkylmethylthiophosphonic acid anhydrides, consisting in that O-alkyl-5-alkylmethylthiophosphonates are reacted with acetyl bromide. The reaction is carried out at 50-60 ° C. Example. A mixture of 26.73 g (0.159 mol) of 0-ethyl-5-ethylmethylthiophosphonate and 8.34 g (0.068 mol) of acetyl bromide is heated to 55-60 ° C for 12 hours. Volatile products are removed, the residue is distilled. Fraction 1: O-ethyl-5-ethylmethylthiophospho-50 ° C / 0, 04 mm, pp (14.56 g) t. 1.4750. The original O-ethyl-3-ethylmethylthiophos 1,4750. Fonat: T. Kin. 65-70 ° С / 1 II fraction: S-ethylmethylthiophosphonic acid anhydride (4.76 g) (54 ° / a from the theoretical) so kin. 120-125 ° C / 0.04 mm, df 1.2563, p 1,5200 MRo 63.42; calculated: 64.22. Found%: C 28.15, 28.40; H 6.00; 6.25; P 24.05; 24.22; S 24.28; 24,69. CeHjgOsPaSa. Calculated,%: C 27.47; H 6.14; P 23.61; S 24.45. Subject of the invention A method for the production of S-alkyl methyl t-phosphonic acid anhydrides, wherein O-alkyl-5-alkyl methyl thiophosphonates are reacted with acetyl bromide at 50-60 ° C.

SU969215A METHOD OF OBTAINING ANHYDRIDES OF 5-ALKYLMETHYLTIO-PHOSPHONE ACIDS SU202943A1 (en)

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SU202943A1 true SU202943A1 (en)

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