SU533584A1 - Method for preparing 4-bromo-2,3,5,6 tetramethylphenol - Google Patents
Method for preparing 4-bromo-2,3,5,6 tetramethylphenolInfo
- Publication number
- SU533584A1 SU533584A1 SU2040973A SU2040973A SU533584A1 SU 533584 A1 SU533584 A1 SU 533584A1 SU 2040973 A SU2040973 A SU 2040973A SU 2040973 A SU2040973 A SU 2040973A SU 533584 A1 SU533584 A1 SU 533584A1
- Authority
- SU
- USSR - Soviet Union
- Prior art keywords
- tetramethylphenol
- bromo
- preparing
- bromine
- yield
- Prior art date
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Description
Изобретение относитс к области получени галоидироваиных фенолов, в ч.астности к усоввршенстваваМНому способу .получени 4-;5:ро.м-2,3,5,6-тетраметилфе.нола, который может быть использован дл получени полиф енил еноксидов.The invention relates to the field of production of halogenated phenols, in particular, to the improvement of the advanced method for obtaining 4-; 5: ro.m-2,3,5,6-tetramethylphenol, which can be used to obtain polyphenyl enoxide.
Известен способ получени 4-бром-2,3,5,6тетраметилфенОЛа обработкой алкилпроизводного фвнола-2,3,5,6-тетра метилфенала бромом в присутствии органического растворител сначала -при ко-миатной температуре в течение 1,5-2 час, с 1последующи;м нагреванием до 60° С. Целевой продукт выдел ют и очищают мристаллизацией, выход ш.родукта 55%A known method for producing 4-bromo-2,3,5,6 tetramethylphenol by treating an alkyl derivative of fvnol-2,3,5,6-tetra methylphenol with bromine in the presence of an organic solvent, first, at a cosmic temperature for 1.5-2 hours, with 1 subsequent heating to 60 ° C. The desired product is isolated and purified by crystallization, the product yield is 55%
1 Недостатками известного способа вл ют-с невысокий выход целбвого продукта, труднодостулность И1СХО|ДНОГО сырь , его высока стоимость,1 The disadvantages of this method are, with a low yield of a curative product, the hardness of I1CHO | BOTH raw materials, its high cost,
С целью повышени выхода целевого продукта |И расшире1ни ассортимента сырь пред .лож-ено в качестве алкиллроизводного фенола использовать 1пентаметилфе;нол и процесс вести три 40-50° С. Исходный печтаметилфеиол может быть лепко получен взаимодействием фенола .с метанолом или лигнина с метанолом и окисью кальци .In order to increase the yield of the target product | And to expand the range of raw materials, it was proposed to use 1 pentamethyl as an alkyl-derivative phenol; nol and the process should be carried out at three 40-50 ° C. calcium oxide.
Процесс ведут в трисутстаии органического растворител , на при1мер уксусной 1кислоты,The process is carried out in trisutsiya organic solvent, for example, acetic acid 1,
н.чи г/;ег-бутилового спирта, или водного ацетан а.n.ch g /; er-butyl alcohol, or aqueous acetone a.
Прн.мер 1. К раствору 32,8 г (0,2 моль) пентаметилфенола в 60 мл 80%-ной ук:усной кислоты :при 40° С прибавл ют за 20 мин 20,7 мл (0,4 моль) брома, лосле чего реакщь Онлую смесь перемешивают 3 час при 40-50° С. Выливанием реакционной смеси в воду получают 41,2 г (90%) 4-бром-2,3,5,6-тетраметилфенола; т. пл. 117-118° С (из летролейного эфира).PRM 1. To a solution of 32.8 g (0.2 mol) of pentamethylphenol in 60 ml of 80% acetic acid: saturated acid: at 40 ° C, 20.7 ml (0.4 mol) of bromine are added in 20 minutes The reaction mixture is stirred for 3 hours at 40-50 ° C. By pouring the reaction mixture into water, 41.2 g (90%) of 4-bromo-2,3,5,6-tetramethylphenol are obtained; m.p. 117-118 ° C (from letrolean ether).
П р и м ер 2. К раствору 1,0 г (6,75 моль) 2,3,5,6-тетраметилфенола в 28 мл лед ной уксусной кислоты прибавл ют 0,35 мл (6,75моль ) брома и выдерживают, перемешива при комнатной температуре, 1,5 час. Затем реакционную смесь -нагревают за 0,5 час до 60° С и выливают в воду.Example 2. To a solution of 1.0 g (6.75 mol) of 2,3,5,6-tetramethylphenol in 28 ml of glacial acetic acid was added 0.35 ml (6.75 mol) of bromine and incubated stirring at room temperature, 1.5 hours. Then the reaction mixture is heated for 0.5 hour to 60 ° C and poured into water.
Получают 1,32 г продукта с т. пл. 100- 110° С, содержащего около 90% 4-бром-2,3,5,6тетраметилфенола . После кристаллизации из пстролейного эфира получают 0,85 г (55%) целевого продукта с т. пл. 118° С.Obtain 1.32 g of product with so pl. 100-110 ° C, containing about 90% 4-bromo-2,3,5,6 tetramethylphenol. After crystallization from pstroleic ether, 0.85 g (55%) of the desired product is obtained with a mp. 118 ° C
Claims (1)
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
SU2040973A SU533584A1 (en) | 1974-06-28 | 1974-06-28 | Method for preparing 4-bromo-2,3,5,6 tetramethylphenol |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
SU2040973A SU533584A1 (en) | 1974-06-28 | 1974-06-28 | Method for preparing 4-bromo-2,3,5,6 tetramethylphenol |
Publications (1)
Publication Number | Publication Date |
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SU533584A1 true SU533584A1 (en) | 1976-10-30 |
Family
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Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
SU2040973A SU533584A1 (en) | 1974-06-28 | 1974-06-28 | Method for preparing 4-bromo-2,3,5,6 tetramethylphenol |
Country Status (1)
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SU (1) | SU533584A1 (en) |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4740636A (en) * | 1986-04-30 | 1988-04-26 | The Dow Chemical Company | Di-ortho-substituted di-meta-halogenated para-halomethylphenols |
-
1974
- 1974-06-28 SU SU2040973A patent/SU533584A1/en active
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4740636A (en) * | 1986-04-30 | 1988-04-26 | The Dow Chemical Company | Di-ortho-substituted di-meta-halogenated para-halomethylphenols |
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