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公开(公告)号:US4486611A
公开(公告)日:1984-12-04
申请号:US412643
申请日:1982-08-30
摘要: A process for the isolation of a dihydroxybenzene-monoether from a reaction mixture containing solvent, ether and unreacted dihydroxybenzene, comprising contacting the reaction mixture with at least one hydrocarbon which is not miscible or only partially miscible with the reaction mixture, the ether selectively entering the hydrocarbon. Advantageously the reaction for the preparation of the monoether is carried out in an alcohol, a ketone, a dipolar aprotic solvent or a polyhydroxyalkyl ether, or a mixture thereof with water, the hydrocarbon used as extracting agent has a boiling point between about 80.degree. and 300.degree. C., and the extraction is carried out in the presence of water whereby there is an increase in the selectivity of the extraction.
摘要翻译: 一种从含有溶剂,醚和未反应的二羟基苯的反应混合物中分离二羟基苯 - 单醚的方法,包括使反应混合物与至少一种与反应混合物不混溶或仅部分混溶的烃接触,所述醚选择性地进入 烃。 有利地,用于制备单醚的反应在醇,酮,偶极非质子溶剂或多羟基烷基醚或其与水的混合物中进行,用作萃取剂的烃的沸点在约80℃和 300℃,萃取在水的存在下进行,由此萃取的选择性增加。
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2.
公开(公告)号:US4321204A
公开(公告)日:1982-03-23
申请号:US170443
申请日:1980-07-21
CPC分类号: C07C43/23 , C07D307/86
摘要: In the preparation of a 7-hydroxycoumaran of the formula ##STR1## in which Z is a hydrogen atom or a substituent which is inert under the subsequent reaction conditions,R.sup.1 is a hydrogen atom or a C.sub.1 to C.sub.4 -alkyl radical, andn is 1, 2 or 3wherein a pyrocatechol of the formula ##STR2## is reacted with an allyl compound of the formula ##STR3## in which Y is a halogen atom, a C.sub.1 to C.sub.4 -alkyl-sulphonate radical or an aryl-sulphonate radical,to form the mono-ether of the pyrocatechol in a first stage, and in a second stage, of the pyrocatechol monoether formed in the first stage is rearranged to a 3-alkenylpyrocatechol, and in a third stage the 3-alkenylpyrocatechol formed in the second stage, is cyclized, the improvement which comprises stages. (b) carrying out the second stage at a pH of about 2-8. Advantageously glycol monomethyl ether is employed as the solvent in all stages and the third stage is carried out with a residence time of about 1-30 minutes and with a narrow residence time spectrum corresponding to a Bodenstein-index 5, optionally in the presence of an iron salt.
摘要翻译: 在制备其中Z为氢原子的式“IMAGE”的7-羟基香豆素或在随后的反应条件下为惰性的取代基时,R 1为氢原子或C 1至C 4 - 烷基,n为 1,2或3其中式IMAMA的邻苯二酚与其中Y是卤素原子,C1-C4烷基磺酸根基或芳基 - 磺酸根基团的式“IMAGE”的烯丙基化合物反应, 在第一阶段中形成邻苯二酚的单醚,在第二阶段将第一阶段中形成的邻苯二酚单醚重新排列为3-链烯基邻苯二酚,第三阶段中形成的3-链烯基邻苯二酚 阶段,循环,改进包括阶段。 (b)在约2-8的pH下进行第二阶段。 在所有阶段中,优选使用二醇单甲醚作为溶剂,第三阶段以约1-30分钟的停留时间和对应于博登斯坦指数5的窄停留时间光谱进行,任选地在 铁盐
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3.
公开(公告)号:US4647676A
公开(公告)日:1987-03-03
申请号:US612962
申请日:1984-05-23
IPC分类号: C07C41/16 , C07C41/38 , C07C43/23 , C07D307/86
摘要: A process for the isolation of a dihydroxybenzenemonoether from a reaction mixture containing solvent, ether and unreacted dihydroxybenzene, comprising contacting the reaction mixture with at least one hydrocarbon which is not miscible or only partially miscible with the reaction mixture, the ether selectively entering the hydrocarbon. Advantageously the reaction for the preparation of the monoether is carried out in an alcohol, a ketone, a dipolar aprotic solvent or a polyhydroxyalkyl ether, or a mixture thereof with water, the hydrocarbon used as extracting agent has a boiling point between about 80.degree. and 300.degree. C., and the extraction is carried out in the presence of water whereby there is an increase in the selectivity of the extraction.
摘要翻译: 一种从含有溶剂,醚和未反应的二羟基苯的反应混合物中分离出二羟基苯氰醚的方法,包括使反应混合物与至少一种与反应混合物不混溶或仅部分混溶的烃接触,醚选择性地进入烃。 有利地,用于制备单醚的反应在醇,酮,偶极非质子溶剂或多羟基烷基醚或其与水的混合物中进行,用作萃取剂的烃的沸点在约80℃和 300℃,萃取在水的存在下进行,由此萃取的选择性增加。
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公开(公告)号:US4383126A
公开(公告)日:1983-05-10
申请号:US315126
申请日:1981-10-26
申请人: Gerhard Buttner , Artur Judat , Udo Allenbach , Manfred Lenthe
发明人: Gerhard Buttner , Artur Judat , Udo Allenbach , Manfred Lenthe
CPC分类号: C07C41/16
摘要: A process for the preparation of a monoalkyl ether of a hydroxyphenol of the formula ##STR1## in which Z each independently is hydrogen or a substituent which is stable under the reaction conditions,R is lower alkyl, andn is 1, 2, 3 or 4,comprising reacting a hydroxyphenol of the formula ##STR2## with an alkyl halide, alkyl sulphonate or aryl sulphonate alkylating agent of the formulaR--Xin which X is a halogen atom, or an alkylsulphonyloxy or arylsulphonyloxy radical,at a temperature from about 130.degree. C. to 200.degree. C. and in the presence of an alkali metal base or alkaline earth metal base and of a diluent comprising a polyhydroxyalkyl ether having at least one OH group. Advantageously the base is sodium carbonate, sodium bicarbonate, potassium carbonate or potassium bicarbonate, the hydroxyphenol is pyrocatechol, the alkylating agent is isopropyl chloride, isopropyl C.sub.1-4 -alkyl-1-sulphonate, isopropyl benzenesulphonate or isopropyl tolyenesulphonate, and the polyhydroxyalkyl ether is glycol monomethyl ether, about 1.5 to 1.8 mols of alkylating agent and about 1 to 2 mols of the base being employed per mol of pyrocatechol, about 1.5 to 2.5 parts by weight of the glycol monomethyl ether being employed per part by weight of pyrocatechol, the reaction being effected in an inert atmosphere under elevated pressure.
摘要翻译: 制备式“IMAGE”的羟基苯酚的单烷基醚的方法,其中Z各自独立地为氢或在反应条件下稳定的取代基,R为低级烷基,n为1,2,3或 4,包括使式(ⅩⅧ)的羟基苯酚与其中X为卤素原子的式RX的烷基卤化物,烷基磺酸盐或芳基磺酸盐烷基化剂或烷基磺酰氧基或芳基磺酰氧基在约130℃ 在碱金属碱或碱土金属碱和包含具有至少一个OH基团的多羟基烷基醚的稀释剂的存在下进行。 有利地,碱是碳酸钠,碳酸氢钠,碳酸钾或碳酸氢钾,羟基苯酚是邻苯二酚,烷基化剂是异丙基氯,异丙基C 1-4 - 烷基-1-磺酸酯,异丙基苯磺酸酯或异丙基甲苯磺酸酯,多羟基烷基醚是 二醇单甲醚,约1.5-1.8摩尔烷基化剂和每摩尔邻苯二酚使用约1-2摩尔的碱,每重量份邻苯二酚使用约1.5-2.5重量份的二醇单甲醚, 反应在惰性气氛中在升高的压力下进行。
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