SU219598A1 - METHOD OF OBTAINING N- (DIALKYLFOCFOChACETIL) FEHOKZAHA - Google Patents
METHOD OF OBTAINING N- (DIALKYLFOCFOChACETIL) FEHOKZAHAInfo
- Publication number
- SU219598A1 SU219598A1 SU1148222A SU1148222A SU219598A1 SU 219598 A1 SU219598 A1 SU 219598A1 SU 1148222 A SU1148222 A SU 1148222A SU 1148222 A SU1148222 A SU 1148222A SU 219598 A1 SU219598 A1 SU 219598A1
- Authority
- SU
- USSR - Soviet Union
- Prior art keywords
- obtaining
- fehokzaha
- dialkylfocfochacetil
- phenoxazine
- product
- Prior art date
Links
- TZMSYXZUNZXBOL-UHFFFAOYSA-N Phenoxazine Chemical compound C1=CC=C2NC3=CC=CC=C3OC2=C1 TZMSYXZUNZXBOL-UHFFFAOYSA-N 0.000 description 4
- 125000002777 acetyl group Chemical group [H]C([H])([H])C(*)=O 0.000 description 3
- BDZBKCUKTQZUTL-UHFFFAOYSA-N Triethyl phosphite Chemical compound CCOP(OCC)OCC BDZBKCUKTQZUTL-UHFFFAOYSA-N 0.000 description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- 238000002955 isolation Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- -1 (bromoacetyl) phenoxazine Chemical compound 0.000 description 1
- BCHZICNRHXRCHY-UHFFFAOYSA-N 2H-oxazine Chemical compound N1OC=CC=C1 BCHZICNRHXRCHY-UHFFFAOYSA-N 0.000 description 1
- RDHPKYGYEGBMSE-UHFFFAOYSA-N Bromoethane Chemical compound CCBr RDHPKYGYEGBMSE-UHFFFAOYSA-N 0.000 description 1
- XDRKCOCUHUAERT-UHFFFAOYSA-N CCCOP([O-])[O-] Chemical compound CCCOP([O-])[O-] XDRKCOCUHUAERT-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 125000005179 haloacetyl group Chemical group 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 239000011541 reaction mixture Substances 0.000 description 1
- 238000001953 recrystallisation Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000002194 synthesizing Effects 0.000 description 1
Description
Изобретение относитс к области получени соединений, которые могут найти применение Б качестве промежуточных продуктов в производстве физиологически активных веществ.The invention relates to the field of the preparation of compounds which can be used as intermediate products in the production of physiologically active substances.
Предлагаемый способ получени Ы-(диалкилфосфонацетил ) - феноксазина заключаетс во взаимодействии расплавленного N- (алоидацетил) феноксазина с триалкилфосфитом при нагревании до 120-140°С с последующим выделением продукта известным способом.The proposed method for the preparation of N- (dialkylphosphone acetyl) -phenoxazine involves the interaction of molten N- (aloidacetyl) phenoxazine with trialkylphosphite when heated to 120-140 ° C, followed by isolation of the product in a known manner.
Пример 1. Получение (диэтилфосфонацетил ) феноксазина.Example 1. Obtaining (diethylphosphone acetyl) phenoxazine.
К 3,05 г расплавленного К-(бромацетил) феноксазина прикапывают 4 г (избыток 2,34 г) триэтилфосфита. Реакционную смесь нагревают 2 час при 120-140°С. Бромистый этил и избыток триэтилфосфита отгон ют в вакууме. В остатке густа жидкость, котора закристаллизовываетс через сутки. Выход продукта после трехкратной перекристаллизации из петролейного эфира 2,3 г (64%), т, пл. 124-126°С.To 3.05 g of molten K- (bromoacetyl) phenoxazine, 4 g (an excess of 2.34 g) of triethyl phosphite are added dropwise. The reaction mixture is heated for 2 hours at 120-140 ° C. Ethyl bromide and excess triethyl phosphite are distilled off in vacuo. The residue is a thick liquid that crystallizes in a day. The yield of the product after three times recrystallization from petroleum ether, 2.3 g (64%), t, pl. 124-126 ° C.
CisHaaNOsP.CisHaaNOsP.
Найдено, о/„: С 60.20; 60,22; Н 5,78; 5,70; N 3,77; 4,08; Р 8,28; 8,32.Found, o / „: C 60.20; 60.22; H 5.78; 5.70; N 3.77; 4.08; P 8.28; 8.32.
Вычислено, о/о; С 59,79; Н 5,54; N 3,88; Р 8,58.Calculated o / o; C, 59.79; H 5.54; N 3.88; R 8.58.
При м ер 2. М-(дипропилфосфонацетил)фен оксазин.At a m er 2. M- (dipropylphosphonacetyl) fen oxazine.
Метод синтеза аналогичен выщеописанному. Из 1,52 г (бромацетил) феноксазина и 1,5 г (избыток 0,46 г) пропилфосфита получают 1,2 г (61,5о/о) продукта с т. пл. 73-75°С.The method of synthesis is similar to that described above. From 1.52 g of (bromoacetyl) phenoxazine and 1.5 g (an excess of 0.46 g) of propyl phosphite, 1.2 g (61.5 ° / o) of product are obtained with a melting point of 200 g. 73-75 ° C.
CosHsjNOsP.CosHsjNOsP.
Найдено, . р 8,15; 7,95; iN 3,92; 3,83.Found p 8.15; 7.95; iN 3.92; 3.83.
Вычислено, %: Р 7,96; N 3,62.Calculated,%: P 7.96; N 3.62.
1515
Предмет изобретени Subject invention
Способ получени Л-(диалкилфосфонацетил )феноксазина, отличающийс тем, что М- (галоидацетил) феноксазин обрабатывают триалкилфосфитом при нагревании до 120- 140°С с последующим выделением продукта известным способом.A method for producing L- (dialkylphosphone acetyl) phenoxazine, wherein M- (haloacetyl) phenoxazine is treated with trialkylphosphite when heated to 120-140 ° C, followed by isolation of the product in a known manner.
Publications (1)
| Publication Number | Publication Date |
|---|---|
| SU219598A1 true SU219598A1 (en) |
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