SU255275A1 - METHOD OF OBTAINING a-TOKOFERIL-OR (-AXEROFTHOL) NICOTINATE - Google Patents
METHOD OF OBTAINING a-TOKOFERIL-OR (-AXEROFTHOL) NICOTINATEInfo
- Publication number
- SU255275A1 SU255275A1 SU1233189A SU1233189A SU255275A1 SU 255275 A1 SU255275 A1 SU 255275A1 SU 1233189 A SU1233189 A SU 1233189A SU 1233189 A SU1233189 A SU 1233189A SU 255275 A1 SU255275 A1 SU 255275A1
- Authority
- SU
- USSR - Soviet Union
- Prior art keywords
- nicotinate
- tokoferil
- axerofthol
- obtaining
- nitrogen
- Prior art date
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- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
Description
Изобретение относитс к области получени соединений, которые могут найти применение в фармацевтической промышленности.The invention relates to the field of the preparation of compounds which can be used in the pharmaceutical industry.
Предлагаемый способ получени а-токоферил-или (-аксерофтол) никотината заключаетс в том, что метиловый эфир никотиновой кислоты нагревают до 60--70°С с ацетатом токоферола или витамина А в токе азота в присутствий метилата натри .The proposed method for the production of α-tocopheryl or (α-asperft) nicotinate is that nicotinic acid methyl ester is heated to 60--70 ° C with tocopherol acetate or vitamin A in a stream of nitrogen in the presence of sodium methoxide.
Пример 1. Получение а-токоферилиикотината .Example 1. Preparation of a-tocopheryl nicotinate.
47,2г (0,1 жолб) а-токоферолацетата и13,7г (0,1 моль) метилового эфира никотиновой кислоты нагревают 2,5 час при 60°С в токе азота , интенсивно перемешива . Затем прибавл ют 1 мл метилата натри и продолжают нагревать ,пр;И 60° С еще 2 час. По окончаНни реакции массу охлаждают, раствор ют в 150 мл н-гексана, раствор промывают всцой до нейтральной: реакции и сушат сер.нокислым натрием.47.2 g (0.1 jolb) of a-tocopherol acetate and 13.7 g (0.1 mol) of nicotinic acid methyl ester are heated for 2.5 hours at 60 ° C in a stream of nitrogen, stirring vigorously. Then 1 ml of sodium methylate is added and heating is continued, etc., and 60 ° C for another 2 hours. At the end of the reaction, the mass is cooled, dissolved in 150 ml of n-hexane, the solution is washed with neutral water until neutral: the reaction is dried with sodium sulfate.
Полученное вещество раствор ют в 50 мл н-гексана и пропускают через колонку с окисью алюмиви (активность П), элюируют н-гексаном . После концентрировани фракций получают 27,55 г (51,6f/o или 57,9% на прореагировавщий а-токоферолацетат).The resulting material is dissolved in 50 ml of n-hexane and passed through a column of alumyum oxide (activity II), eluted with n-hexane. After concentration of the fractions, 27.55 g (51.6 f / o or 57.9% for the reacted a-tocopherol acetate) are obtained.
Вычислено, о/о: С 78,38; Н 9, 89; N 2,61. CssHsaOsN.Calculated, o / o: C 78.38; H 9, 89; N 2.61. CssHsaOsN.
Найдено, %: С 78,80; Н .10,70; N 2,79.Found,%: C 78.80; H.10.70; N 2.79.
При.мер 2. Получение аксерофтолни1котината .Ex. 2. Receipt of akerofolny1kotinat.
5 г (0,0152 моль) ацетата витамина А и 2,09 г (0,0152 моль) метилового эфира никотиновой кислоты нагревают при 60-65°С в течение 1,5 час в токе азота, после чего прибавл ют 0,25 мл металата натри и в тех же услови х провод т реакцию еще 1,5 час.5 g (0.0152 mol) of vitamin A acetate and 2.09 g (0.0152 mol) of nicotinic acid methyl ester are heated at 60-65 ° C for 1.5 hours in a stream of nitrogen, after which 0.25 is added. ml of sodium metalate and under the same conditions, the reaction is carried out for another 1.5 hours.
Реакционную смесь раствор ют в 50 л«л н-гексана, промывают водой (150 мл) и сушат сернокислым натрием в азоте. Полученный раствор пропускают через колонку с окисью алюми и (активность П) в токе азота , элюируют н-гексаном.The reaction mixture is dissolved in 50 liters of l-n-hexane, washed with water (150 ml) and dried with sodium sulfate in nitrogen. The resulting solution is passed through a column with alumina and (activity P) in a stream of nitrogen, eluted with n-hexane.
После концентрировани фракций получают 3,94 г (66,1% или 820/0 на вступивший в реакцию витамин А-ацетат) вещества, df 1,1304; n, 1,6123; MRp: найдено 120,30, вычислено 120,56.After concentrating the fractions, 3.94 g (66.1% or 820/0 per reacted vitamin A acetate) of the substance, df 1.1304, are obtained; n, 1.6123; MRp: found 120.30, calculated 120.56.
Вычислено, %: С 79,79; Н 8,44; N 3,58. 3 Предмет изобретени Спосаб получени а-то,коферил- или (-аксерофтол ) никотината, отличающийс тем, что метиловый эфир никотиновой кислоты нагре- 5 4 вают до 60-70 С с ацетатом токоферола или вита1мина А в азота в присустствии метнлата натри с П0;сл0дуюш.им выделением целевого лродукта иэвест1ным способоМ.Calculated,%: C 79.79; H 8.44; N 3.58. 3 Subject of the invention: Sposab of preparing a, coferyl- or (-axeroftol) nicotinate, characterized in that methyl nicotinic acid ester is heated to 60-70 ° C with tocopherol or vitamin A acetate in nitrogen in the presence of sodium methlate from O ; by the selection of the target product by the well-known method.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
SU1233189A SU255275A1 (en) | 1968-04-09 | 1968-04-09 | METHOD OF OBTAINING a-TOKOFERIL-OR (-AXEROFTHOL) NICOTINATE |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
SU1233189A SU255275A1 (en) | 1968-04-09 | 1968-04-09 | METHOD OF OBTAINING a-TOKOFERIL-OR (-AXEROFTHOL) NICOTINATE |
Publications (1)
Publication Number | Publication Date |
---|---|
SU255275A1 true SU255275A1 (en) | 1973-05-25 |
Family
ID=20442270
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
SU1233189A SU255275A1 (en) | 1968-04-09 | 1968-04-09 | METHOD OF OBTAINING a-TOKOFERIL-OR (-AXEROFTHOL) NICOTINATE |
Country Status (1)
Country | Link |
---|---|
SU (1) | SU255275A1 (en) |
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1968
- 1968-04-09 SU SU1233189A patent/SU255275A1/en active
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