SU466232A1 - The method of obtaining condensed pyrimido-triazinium compounds with bridging nitrogen atoms - Google Patents

The method of obtaining condensed pyrimido-triazinium compounds with bridging nitrogen atoms

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Publication number
SU466232A1
SU466232A1 SU1924689A SU1924689A SU466232A1 SU 466232 A1 SU466232 A1 SU 466232A1 SU 1924689 A SU1924689 A SU 1924689A SU 1924689 A SU1924689 A SU 1924689A SU 466232 A1 SU466232 A1 SU 466232A1
Authority
SU
USSR - Soviet Union
Prior art keywords
pyrimido
nitrogen atoms
bridging nitrogen
obtaining condensed
compounds
Prior art date
Application number
SU1924689A
Other languages
Russian (ru)
Inventor
Виталий Афанасьевич Чуйгук
Константин Владимирович Федотов
Original Assignee
Киевский Ордена Ленина Государственный Университет Им.Т.Г.Шевченко
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.)
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Application filed by Киевский Ордена Ленина Государственный Университет Им.Т.Г.Шевченко filed Critical Киевский Ордена Ленина Государственный Университет Им.Т.Г.Шевченко
Priority to SU1924689A priority Critical patent/SU466232A1/en
Application granted granted Critical
Publication of SU466232A1 publication Critical patent/SU466232A1/en

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  • Nitrogen Condensed Heterocyclic Rings (AREA)

Description

„ „ н СГзСООН C CH-C-B + Rj -C-C-Rj „„ Mr. SGSC CH-C-B + Rj-C-C-Rj

ОABOUT

RiRi

NHj NHj

NN HOI + R - С - CH - С - R + I/N,NN HOI + R - C - CH - C - R + I / N,

CF.COOH RCF.COOH R

I 1 I I 1 I

, ,

Целевые продукты выдел ют из1вестныМИ гриемами.Target products are isolated from known greems.

П р и-М е 1р 1. 7,9-Д|И|Мет1ил-2,3-дифенилпиримидо- (1,2: 1,5)-з-триазоло - {4,3-Ь - as-триазиний перхло-рат.P p i-M e 1p 1. 7,9-D | I | Methyl-2,3-diphenylpyrimido- (1,2: 1,5) -z-triazolo - {4,3-b - as-triazine perchlo -Ret

Смесь 1 г бром-гидрата гуаназина, 1 мл ацетилацетона и 1,4 г беизилл з 2 мл трифторуксусной -кислоты нагревают 3 час с обратным холодильникам на масл ной бане при 145° С. После охлаждени  реакционную смесь выливают в мл эфира, растирают с эфиром и отфильтровывают 2,5 г (79%) трифторацетата , который превращают в перхлорат добавлением 57 %-иого. раствора хлорной кислоты . Температура плавлени  (перхлората 288 С (н-итрометан).A mixture of 1 g of guanazine bromine hydrate, 1 ml of acetylacetone and 1.4 g of beisillus with 2 ml of trifluoroacetic a-acid is heated for 3 hours with refluxing refrigerators in an oil bath at 145 ° C. After cooling, the reaction mixture is poured into ml of ether, triturated with ether and filter 2.5 g (79%) of trifluoroacetate, which is converted to perchlorate by adding 57%. perchloric acid solution. Melting point (perchlorate 288 C (n-itromethane).

Найдена, %: С1 7,5.Found%: C1 7.5.

C2lH,7ClN604.C2lH, 7ClN604.

Вычислено, %: С1 7,8.Calculated,%: C1 7.8.

Пример 2. 2,3,8,10-тетраметилииримидо (Г , 1,5)-з-Т1риазоло - (3,4 : 1,5-8-триазоло 4 ,3-Ь -а5-триазиний .перхлорат.Example 2. 2,3,8,10-tetramethylirimido (G, 1,5) -z-T1riazolo - (3.4: 1.5-8-triazolo 4, 3-b-a5-triazino. Perchlorate.

Смесь хлоргидрата 3,6,7-триамино-7Н-5трН1азоло- 5 ,1-с -з-трИазола, 1 мл ацетилацетона ,и 0,6 мл диацетила в 5 мл тр«фтаруксусной кислоты нагревают 2 час «а масл ной бане с обратным холодильником при 130° С, после |чего обрабатывают по примеру 1. Выход 1,4 г (70%); т. пл: 25ГС (с разл.).A mixture of 3,6,7-triamino-7H-5trH1azolo-5, 1-c-z-trIazole hydrochloride, 1 ml of acetylacetone, and 0.6 ml of diacetyl in 5 ml of tr "phtharoacetic acid is heated for 2 hours in an oil bath with reflux at 130 ° C, after which it is treated as in example 1. Yield 1.4 g (70%); m.p .: 25GS (with different).

Пайдено, %: С1 9,6.Paydeno,%: C1 9.6.

; Я ; I

R,R,

C,2H,.C, 2H ,.

Вычислено, %: С1 9,6.Calculated,%: C1 9.6.

Пример 3. 8,10-диметил-2,3-дифенилтшримидо- (1,2 : 1,5) - s - трвазоло-(3,4 : 1,5)-sтриазоло- 4 ,3-Ь -а5-тр азищий перхлорат.Example 3. 8,10-dimethyl-2,3-diphenylsrimido- (1.2: 1.5) - s - trzazolo- (3.4: 1.5) -triazolo- 4, 3-b-a5-tr Asian perchlorate.

Это соединение получают аналогично примеру 2 из 3,6,7-триам:ино-7Н-з-11риазоло- 5,1-с з-триазола , ацетилацетона и бензила при вагревании в течение 2,5 час при 120° С.This compound is prepared analogously to example 2 of 3,6,7-triam: foreign-7H-3-11riazolo-5,1-C 3-triazole, acetylacetone and benzyl during heating for 2.5 hours at 120 ° C.

.Выход 63%, т. пл. 191°С (с разл.) (этанол - нитрометаи)..Outlet 63%, so pl. 191 ° C (with decomp.) (Ethanol - nitrometai).

Найдено: %; С1 7,4; N 22,3.Found:%; C1 7.4; N 22.3.

C22H,sCl:N804.C22H, sCl: N804.

Вычислено, %: С1 7,2; N 22,8.Calculated,%: C1 7.2; N 22.8.

Предмет и з о -б р е т е и и  Subject and s about-and r and and

Claims (2)

1.Способ получени  конденсированных пиримидо-аз-триазиниевых Соединений с мостиковыми атомами азота, отличающийс  тем, что протонированный три-амйноазагетероцикл, в котором две аминогрупиы наход тс  в поло Ж6НИЯХ 1 и 2, причем одна из них св зана с циклическим .атомом азота, а треть  находитс  в «-положении к азаатому, подвергают взаимодействию со смесью а- и р-дикетонов с последующем выделением целевых 1продуктов известными прием-ами.;1. A method of producing condensed pyrimido-az-triazine compounds with bridging nitrogen atoms, characterized in that a protonated tri-amine heterocycle in which two amino groups are located in boxes 6 and 1 and 2, one of which is bound to a cyclic nitrogen atom, and one third is in the "position to the azaatom, and is reacted with a mixture of a- and p-diketones, followed by isolation of the target products by known methods; 2.Способ по п. 1, отличающийс  тем, что процесс провод т при нагрвв-ании в трифторуксусной К1ислоте.2. A method according to claim 1, characterized in that the process is carried out upon heating in trifluoroacetic acid.
SU1924689A 1973-05-23 1973-05-23 The method of obtaining condensed pyrimido-triazinium compounds with bridging nitrogen atoms SU466232A1 (en)

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SU1924689A SU466232A1 (en) 1973-05-23 1973-05-23 The method of obtaining condensed pyrimido-triazinium compounds with bridging nitrogen atoms

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
RU2315053C2 (en) * 2000-05-26 2008-01-20 Шеринг Корпорейшн DERIVATIVES OF 5-AMINOPYRAZOLO-[4,3-e]-1,2,4-TRIAZOLO-[1,5-c]-PYRIMIDINE, PHARMACEUTICAL COMPOSITION BASED ON THEREOF, USING AND METHODS FOR PREPARING INTERMEDIATE COMPOUNDS
CN105254636A (en) * 2015-11-04 2016-01-20 中国工程物理研究院化工材料研究所 3,6,7-triamino-1,2,4-triazolocycle ionic type nitroazole compound and preparation method thereof

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
RU2315053C2 (en) * 2000-05-26 2008-01-20 Шеринг Корпорейшн DERIVATIVES OF 5-AMINOPYRAZOLO-[4,3-e]-1,2,4-TRIAZOLO-[1,5-c]-PYRIMIDINE, PHARMACEUTICAL COMPOSITION BASED ON THEREOF, USING AND METHODS FOR PREPARING INTERMEDIATE COMPOUNDS
CN105254636A (en) * 2015-11-04 2016-01-20 中国工程物理研究院化工材料研究所 3,6,7-triamino-1,2,4-triazolocycle ionic type nitroazole compound and preparation method thereof
CN105254636B (en) * 2015-11-04 2017-10-24 中国工程物理研究院化工材料研究所 Triazol ring ionic nitro azole compounds of 3,6,7 triamido 1,2,4 and preparation method thereof

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