SU466212A1 - The method of obtaining hydrochloric acid salts of 1,5-diamino or 1,3,5,7-tetraminoadamanediol-2,6 - Google Patents

The method of obtaining hydrochloric acid salts of 1,5-diamino or 1,3,5,7-tetraminoadamanediol-2,6

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Publication number
SU466212A1
SU466212A1 SU1922284A SU1922284A SU466212A1 SU 466212 A1 SU466212 A1 SU 466212A1 SU 1922284 A SU1922284 A SU 1922284A SU 1922284 A SU1922284 A SU 1922284A SU 466212 A1 SU466212 A1 SU 466212A1
Authority
SU
USSR - Soviet Union
Prior art keywords
hydrochloric acid
diamino
tetraminoadamanediol
acid salts
obtaining hydrochloric
Prior art date
Application number
SU1922284A
Other languages
Russian (ru)
Inventor
Игорь Константинович Моисеев
Валентина Петровна Коновалова
Original Assignee
Предприятие П/Я В-8413
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Предприятие П/Я В-8413 filed Critical Предприятие П/Я В-8413
Priority to SU1922284A priority Critical patent/SU466212A1/en
Application granted granted Critical
Publication of SU466212A1 publication Critical patent/SU466212A1/en

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Description

20 мл воды. По окончании добавлени  эфирный слой отдел ют, а водный экстрагируют трижды 30 мл эфира. Объединенные эфирные выт жки промывают 2%-ным раствором бикарбоната натри  и водой, после чего сушат над хлористым кальцием. Зфир отгон ют, добавл ют 75 мл сухого хлороформа и кип т т с хлоркальциевой трубкой до прекращени  выделени  азота (1-1,5 час). Далее хлороформ отгон ют, добавл ют 50 мл сол ной кислоты (d 1,17 г/см) и кип т т 1-1,5 час. Выпавшую соль отфильтровывают, маточник упаривают до 1/3 объема и добавочно отфильтровывают соль. Общий вес соли 2,21 г. После высаживани  ацетоном из воды получают 1,9 г (41%) целевого продукта, т. пл. выще 360°С. Содержание основного вещества, определенное потенциометрическим титрованием, 96%.20 ml of water. At the end of the addition, the ether layer is separated and the aqueous layer is extracted three times with 30 ml of ether. The combined ether extracts are washed with 2% sodium bicarbonate solution and water, and then dried over calcium chloride. The zirr is distilled off, 75 ml of dry chloroform is added and boiled with a calcium chloride tube until the evolution of nitrogen ceases (1-1.5 hours). Next, chloroform was distilled off, 50 ml of hydrochloric acid (d 1.17 g / cm) was added and the mixture was boiled for 1-1.5 hours. The precipitated salt is filtered, the mother liquor is evaporated to 1/3 of the volume and the salt is additionally filtered off. The total salt weight is 2.21 g. After precipitating with acetone, 1.9 g (41%) of the desired product is obtained from water, mp. Higher than 360 ° C. The content of the basic substance, determined by potentiometric titration, is 96%.

Найдено, %: С 31,91, 31,59; П 6,17, 6,19; N 149,96, 14,34; С1 37,5, 37,14.Found,%: C 31.91, 31.59; P 6.17, 6.19; N 149.96, 14.34; C1 37.5, 37.14.

CloH24N4Cl4O2.CloH24N4Cl4O2.

Вычислено, %: С 32,08; Н 6,42; N 14,97; С1 37,96.Calculated,%: C 32.08; H 6.42; N 14.97; C1 37.96.

Предмет изобретени Subject invention

Способ получени  сол нокислых солей 1,5диамино- или 1,3,5,7-тетраминоадамантандиола-2 ,6, отличающийс  тем, что соответствующие гидразиды 2,6-диоксиадамантанкарбоновых кислот подвергают взаимодействию с нитритом натри  при температуре не выше 10°С с последующим воздействием на образовавшиес  ацилазиды хлороформом и обработкой полученных изоцианатов сол ной кислотой с выделением целевого продукта в виде сол нокислых солей известным способом.The method of producing hydrochloric acid salts of 1,5-diamino or 1,3,5,7-tetraminoadamantane-2, 6, characterized in that the corresponding hydrazides of 2,6-dioxyadamantane carboxylic acids are reacted with sodium nitrite at a temperature not higher than 10 ° C, followed exposure to the formed acyl azides with chloroform and the treatment of the obtained isocyanates with hydrochloric acid with the isolation of the target product in the form of hydrochloric salts in a known manner.

SU1922284A 1973-05-11 1973-05-11 The method of obtaining hydrochloric acid salts of 1,5-diamino or 1,3,5,7-tetraminoadamanediol-2,6 SU466212A1 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
SU1922284A SU466212A1 (en) 1973-05-11 1973-05-11 The method of obtaining hydrochloric acid salts of 1,5-diamino or 1,3,5,7-tetraminoadamanediol-2,6

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
SU1922284A SU466212A1 (en) 1973-05-11 1973-05-11 The method of obtaining hydrochloric acid salts of 1,5-diamino or 1,3,5,7-tetraminoadamanediol-2,6

Publications (1)

Publication Number Publication Date
SU466212A1 true SU466212A1 (en) 1975-04-05

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Application Number Title Priority Date Filing Date
SU1922284A SU466212A1 (en) 1973-05-11 1973-05-11 The method of obtaining hydrochloric acid salts of 1,5-diamino or 1,3,5,7-tetraminoadamanediol-2,6

Country Status (1)

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SU (1) SU466212A1 (en)

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