Process of producing high purity bis(4-hydroxyphenyl)sulfides and
heat-sensitive recording materials containing the same
    2.
    发明授权
    Process of producing high purity bis(4-hydroxyphenyl)sulfides and heat-sensitive recording materials containing the same 失效
    制备高纯度双(4-羟基苯基)硫化物和含有它们的热敏记录材料的方法

    公开(公告)号:US5175372A

    公开(公告)日:1992-12-29

    申请号:US683554

    申请日:1991-04-10

    CPC分类号: B41M5/3336 C07C319/14

    摘要: In a process of producing high purity bis(4-hydroxyphenyl)sulfides which comprises reacting phenols with sulfur dichloride in an organic solvent, the improvement comprising: reacting the phenols with sulfur dichloride in a nonpolar organic solvent; removing partly or wholly the nonpolar organic solvent after the reaction; adding a polar organic solvent to the reaction mixture to dissolve the reaction mixture therein at elevated temperatures; and crystallizing out the high purity bis(4-hydroxyphenyl)sulfides.There is further provided a high performance heat-sensitive recording material which comprises high purity bis(4-hydroxy-3-methylphenyl)sulfide thus prepared and having a melting point in the range of from 123.9.degree. C. to 124.9.degree. C. as a developer and a fluoran compound as a color former.

    摘要翻译: 在制备高纯度双(4-羟基苯基)硫化物的方法中,其包括在有机溶剂中使酚与二氯化硫反应,其改进包括:使苯酚与二氯化硫在非极性有机溶剂中反应; 反应后部分或全部去除非极性有机溶剂; 向反应混合物中加入极性有机溶剂以在升高的温度下溶解其中的反应混合物; 并结晶出高纯度的双(4-羟基苯基)硫化物。 进一步提供了一种高性能热敏记录材料,其包含如此制备的高纯度双(4-羟基-3-甲基苯基)硫化物,熔点范围为123.9℃至124.9℃,为 显影剂和作为成色剂的荧烷化合物。

    Process for preparing N,N-dialkylaniline salt of 5-acetyl-2-alkylbenzene
sulfonic acid
    4.
    发明授权
    Process for preparing N,N-dialkylaniline salt of 5-acetyl-2-alkylbenzene sulfonic acid 失效
    制备5-乙酰基-2-烷基苯磺酸的N,N-二烷基苯胺盐的方法

    公开(公告)号:US4853158A

    公开(公告)日:1989-08-01

    申请号:US178833

    申请日:1988-03-25

    CPC分类号: C07C309/00

    摘要: Process for preparing 2-alkyl-5-haloacetylbenzenesulfonamide represented by the general formula (1), ##STR1## (wherein R.sup.1 is an alkyl group having 1 to 5 carbon atoms; and X is a chlorine atom, bromine atom or iodine atom), characterized by halogenating a 5-acetyl-2-alkylbenzenesulfonamide represented by the general formula (2), ##STR2## (wherein R.sup.1 is the same as defined above) in a lower alcohol represented by the general formula (3),R.sup.4 --OH(wherein R.sup.4 is an alkyl group having 1 to 5 carbon atoms).

    摘要翻译: 用于制备由通式(1)表示的2-烷基-5-卤代乙酰基苯磺酰胺的方法,其中R1是具有1-5个碳原子的烷基; X是氯原子,溴原子或碘 原子),其特征在于在通式(3)表示的低级醇中卤化由通式(2)表示的5-乙酰基-2-烷基苯磺酰胺,(IMAG)(2)(其中R 1与上述相同) ),R4-OH(其中R4是具有1至5个碳原子的烷基)。

    Thiophene derivatives and methods for producing the same
    5.
    发明授权
    Thiophene derivatives and methods for producing the same 失效
    噻吩衍生物及其制备方法

    公开(公告)号:US4792612A

    公开(公告)日:1988-12-20

    申请号:US171388

    申请日:1988-03-21

    摘要: Novel compounds, 2-(.alpha.-alkoxyimino)ethylthiophenes are susceptible to electrophilic substitution reactions, and the acetylation, nitration, sulfonation and halogenation of the compounds provide 5-acetyl-2-(.alpha.-alkoxyimino)ethylthiophenes, 5-nitro-2-(.alpha.-alkoxyimino)ethylthiophenes, 5-(.alpha.-alkoxyimino)ethyl-2-thiophenesulfonic acid and 5-halo-2-(.alpha.-alkoxyimino)ethylthiophenes, respectively.The hydrolysis of 5-acetyl-2-(.alpha.-alkoxyimino)ethylthiophenes readily provides a known compound, 2,5-diacetylthiophene which is an important intermediate for the production of medicines, whereas the haloform reaction provides novel compounds, 5-(.alpha.-alkoxyimino)ethyl-2-thiophenecarboxylic acids, the hydrolysis of which compounds readily provides a known compound, 5-acetyl-2-thiophenecarboxylic acids, an important intermediate for the production of medicines.The hydrolysis of 5-(.alpha.-alkoxyimino)ethyl-2-thiophenesulfonic acids and their salts provide novel 5-acetyl-2-thiophenesulfonic acid and its salts, respectively.Novel compounds, 2-(.alpha.-alkoxyimino)ethylthiophenes are obtained either by 0-alkylation of 2-acetylthiophene oxime or by directly reacting 2-acetylthiophene with an 0-alkylhydroxylamine.

    摘要翻译: 新化合物2-(α-烷氧基亚氨基)乙基噻吩对亲电取代反应敏感,化合物的乙酰化,硝化,磺化和卤化提供5-乙酰基-2-(α-烷氧基亚氨基)乙基噻吩,5-硝基-2- (α-烷氧基亚氨基)乙基噻吩,5-(α-烷氧基亚氨基)乙基-2-噻吩磺酸和5-卤代-2-(α-烷氧基亚氨基)乙基噻吩。 5-乙酰基-2-(α-烷氧基亚氨基)乙基噻吩的水解容易提供已知的化合物,2,5-二乙酰基噻吩,其是制备药物的重要中间体,而卤代反应提供新化合物5-(α- 烷氧基亚氨基)乙基-2-噻吩羧酸,其中哪些化合物的水解容易提供已知化合物5-乙酰基-2-噻吩羧酸,这是生产药物的重要中间体。 5-(α-烷氧基亚氨基)乙基-2-噻吩磺酸及其盐的水解分别提供新的5-乙酰基-2-噻吩磺酸及其盐。 通过2-乙酰基噻吩肟的O-烷基化或通过使2-乙酰基噻吩与O-烷基羟胺直接反应得到2-(α-烷氧基亚氨基)乙基噻吩的新型化合物。

    Process for producing p-hydroxybenzaldehyde
    7.
    发明授权
    Process for producing p-hydroxybenzaldehyde 失效
    对羟基苯甲醛生产方法

    公开(公告)号:US4273941A

    公开(公告)日:1981-06-16

    申请号:US55414

    申请日:1979-07-06

    IPC分类号: C07C45/64 C07C85/11 C07C89/00

    CPC分类号: C07C45/64

    摘要: A process for producing p-hydroxybenzaldehyde through p-aminobenzaldehyde from p-nitrotoluene, comprising reacting p-nitrotoluene with sodium polysulphide in an alcohol-alkali aqueous solution mixed solvent in the presence or absence of an aprotic polar compound to produce p-aminobenzaldehyde, diazotizing the p-aminobenzaldehyde and then hydrolyzing the diazotized p-aminobenzaldehyde to produce p-hydroxybenzaldehyde.

    摘要翻译: 在对硝基甲苯中通过对氨基苯甲醛生产对羟基苯甲醛的方法,包括在存在或不存在非质子极性化合物的情况下,将对硝基甲苯与多硫化钠在醇 - 碱水溶液混合溶剂中反应生成对氨基苯甲醛,重氮化 对氨基苯甲醛,然后水解重氮化的对氨基苯甲醛以产生对羟基苯甲醛。

    Process for producing p-hydroxybenzaldehyde
    8.
    发明授权
    Process for producing p-hydroxybenzaldehyde 失效
    对羟基苯甲醛生产方法

    公开(公告)号:US4195041A

    公开(公告)日:1980-03-25

    申请号:US938125

    申请日:1978-08-30

    IPC分类号: C07C45/64 C07C45/00

    CPC分类号: C07C45/64

    摘要: A process for producing p-hydroxybenzaldehyde through p-aminobenzaldehyde from p-nitrotoluene, comprising reacting p-nitrotoluene with sodium polysulphide in an alcohol-alkali aqueous solution mixed solvent in the presence or absence of an aprotic polar compound to produce p-aminobenzaldehyde, diazotizing the p-aminobenzaldehyde and then hydrolyzing the diazotized p-aminobenzaldehyde to produce p-hydroxybenzaldehyde.

    摘要翻译: 在对硝基甲苯中通过对氨基苯甲醛生产对羟基苯甲醛的方法,包括在存在或不存在非质子极性化合物的情况下,将对硝基甲苯与多硫化钠在醇 - 碱水溶液混合溶剂中反应生成对氨基苯甲醛,重氮化 对氨基苯甲醛,然后水解重氮化的对氨基苯甲醛以产生对羟基苯甲醛。

    Novel thiophene derivatives and methods for producing the same
    9.
    发明授权
    Novel thiophene derivatives and methods for producing the same 失效
    新型噻吩衍生物及其制备方法

    公开(公告)号:US5101049A

    公开(公告)日:1992-03-31

    申请号:US569540

    申请日:1990-08-20

    摘要: Novel compounds, 2-(.alpha.-alkoxyimino)ethylthiophenes are susceptible to electrophilic substitution reactions, and the acetylation, nitration, sulfonation and halogenation of the compounds provide 5-acetyl-2-(.alpha.-alkoxyimino)ethylthiophenes, 5-nitro-2-(.alpha.-alkoxyimino)ethylthiophenes, 5-(.alpha.-alkoxyimino)ethyl-2-thiophenesulfonic acid and 5-halo-2-(.alpha.-alkoxyimino)ethylthiophenes, respectively.The hydrolysis of 5-acetyl-2-(.alpha.-alkoxyimino)ethylthiophenes readily provides a known compound, 2,5-diacetylthiophene which is an important intermediate for the production of medicines, whereas the haloform reaction provides novel compounds, 5-(.alpha.-alkoxyimino)ethyl-2-thiophenecarboxylic acids, the hydrolysis of which compounds readily provides a known compound, 5-acetyl-2-thiophenecarboxylic acids, an important intermediate for the production of medicines.The hydrolysis of 5-(.alpha.-alkoxyimino)ethyl-2-thiophenesulfonic acids and their salts provide novel 5-acetyl-2-thiophenesulfonic acid and its salts, respectively.Novel compounds, 2-(.alpha.-alkoxyimino)ethylithiophenes are obtained either by 0-alkylation of 2-acetylthiophene oxime or by directly reacting 2-acetylthiophene with an 0-alkylhydroxylamine.

    摘要翻译: 新化合物2-(α-烷氧基亚氨基)乙基噻吩对亲电取代反应敏感,化合物的乙酰化,硝化,磺化和卤化提供5-乙酰基-2-(α-烷氧基亚氨基)乙基噻吩,5-硝基-2- (α-烷氧基亚氨基)乙基噻吩,5-(α-烷氧基亚氨基)乙基-2-噻吩磺酸和5-卤代-2-(α-烷氧基亚氨基)乙基噻吩。 5-乙酰基-2-(α-烷氧基亚氨基)乙基噻吩的水解容易提供已知的化合物,2,5-二乙酰基噻吩,其是制备药物的重要中间体,而卤代反应提供新化合物5-(α- 烷氧基亚氨基)乙基-2-噻吩羧酸,其中哪些化合物的水解容易提供已知化合物5-乙酰基-2-噻吩羧酸,这是生产药物的重要中间体。 5-(α-烷氧基亚氨基)乙基-2-噻吩磺酸及其盐的水解分别提供新的5-乙酰基-2-噻吩磺酸及其盐。 通过2-乙酰基噻吩肟的O-烷基化或通过使2-乙酰基噻吩与O-烷基羟胺直接反应,得到2-(α-烷氧基亚氨基)乙基噻吩类化合物。

    Method of producing alkali metal benzenesulfinates
    10.
    发明授权
    Method of producing alkali metal benzenesulfinates 失效
    制备碱金属苯亚磺酸盐的方法

    公开(公告)号:US4849138A

    公开(公告)日:1989-07-18

    申请号:US84572

    申请日:1987-08-12

    CPC分类号: C07C313/04 C07C317/00

    摘要: A method of producing alkali metal benzenesulfinates having the general formula of ##STR1## wherein M represents Na or K, which comprises: reacting nitrophenylphenyl sulfones having the general formula of ##STR2## wherein n is an integer of 1 or 2, with alkali metal thiophenolates having the general formula of ##STR3## in solvents. The reaction produces also nitrophenylphenyl sulfides as by-products in equimolar amounts to the alkali metal benzenesulfinates, and the oxidation of the sulfides provides the starting nitrophenylphenyl sulfones.A method of producing the nitrophenylphenyl sulfones is also provided wherein the sulfides are oxidized with hydrogen peroxide in the presence both of water-soluble tungstates or molybdates and of phase transfer catalysts in a two-phase heterogeneous solvent.

    摘要翻译: 将通式为“IMAGE”的碱金属苯亚磺酸盐的制备方法,其中M代表Na或K,其中包括:将具有通式“IMAGE”的硝基苯基砜与n = 1或2的整数与碱金属硫代苯酚酯反应 在溶剂中具有的通式。 该反应还产生硝基苯基苯基硫化物作为等摩尔量的碱金属苯亚磺酸盐的副产物,并且硫化物的氧化提供起始的硝基苯基苯砜。 还提供了一种制备硝基苯基苯砜的方法,其中硫化物在水溶性钨酸盐或钼酸盐存在的情况下用过氧化氢氧化,并且在两相非均相溶剂中用相转移催化剂氧化。