Process for the preparation of chloroformic acid aryl esters
    1.
    发明授权
    Process for the preparation of chloroformic acid aryl esters 失效
    氯甲酸芳酯的制备方法

    公开(公告)号:US4366102A

    公开(公告)日:1982-12-28

    申请号:US261082

    申请日:1981-05-06

    摘要: In a process for the preparation of an aromatic chloroformic acid ester by contacting a phenol and phosgene, the improvement wherein the reaction is carried out in a homogeneous liquid phase at a temperature of 60.degree. to 180.degree. C. in the presence of organic phosphorus compound of the formulaR.sup.1 R.sup.2 R.sup.3 PR.sup.4.sub.n X.sub.nin whichR.sup.1, R.sup.2 and R.sup.3 independently of one another represent hydrogen, alkyl, alkenyl, aralkyl, aryl or halogen and two of the said radicals together with the phosphorus atom can form a 5-membered or 6-membered phosphorus-containing saturated or unsaturated heterocyclic radical,X represents OH, homopolar-bonded halogen or an inorganic or organic acid anion,R.sup.4 denotes hydrogen or alkyl or, if X denotes halogen, can also denote halogen and n denotes 0 or 1,and in which, furthermore,R.sup.4 and X together can represent oxygen or sulfur.

    摘要翻译: 在通过使苯酚和光气接触来制备芳族氯甲酸酯的方法中,其中反应在有机磷化合物存在下在60-180℃的温度下在均相液相中进行 其中R 1,R 2和R 3彼此独立地表示氢,烷基,烯基,芳烷基,芳基或卤素,并且所述基团中的两个与磷原子一起形成式R 1 R 2 R 3 PR 4 n X n可以形成5元或6元磷 - 含有饱和或不饱和杂环基,X表示OH,单键键合的卤素或无机或有机酸阴离子,R4表示氢或烷基,或者如果X表示卤素,也可以表示卤素,n表示0或1, 此外,R4和X可以一起代表氧或硫。

    Process for the preparation of 1,5-dihydroxynaphthalene and
1,5-diaminonaphthalene
    4.
    发明授权
    Process for the preparation of 1,5-dihydroxynaphthalene and 1,5-diaminonaphthalene 失效
    制备1,5-二羟基萘和1,5-二氨基萘的方法

    公开(公告)号:US4973758A

    公开(公告)日:1990-11-27

    申请号:US439757

    申请日:1989-11-21

    摘要: The characteristic of the improved process for the preparation of 1,5-dihydroxynaphthalene and 1,5-diaminonaphthalene is to carry out the alkaline pressure hydrolysis of the disodium salt of naphthalene-1,5-disulphonic acid at temperatures from 270.degree. to 290.degree. C. and under 14 to 20 bar using an excess of sodium hydroxide solution such that the molar ratio NaOH/disodium salt of naphthalenesulphonic acid is at least 12:1. The 1,5-dihydroxynaphthalene which is obtained in this manner, without hazard and in substantially higher purity, is then aminated with ammonia in the presence of ammonium bisulphite to give 1,5-diaminonaphthalene, it being possible to achieve a further increase in the degree of purity of the 1,5-diaminonaphthalene by increasing the molar ratio NH.sub.3 /1,5-dihydroxynaphthalene to at least 6:1.

    摘要翻译: 制备1,5-二羟基萘和1,5-二氨基萘的改进方法的特点是在270〜290℃的温度下进行萘-1,5-二磺酸二钠盐的碱性水解 并使用过量的氢氧化钠溶液使14至20巴,使得萘磺酸的NaOH /二钠盐的摩尔比至少为12:1。 然后用亚硫酸铵存在下用氨将胺化得到的1,5-二羟基萘没有危害并且纯度高得多,得到1,5-二氨基萘,可以进一步增加 通过将NH 3 / 1,5-二羟基萘的摩尔比提高到至少6:1,1,5-二氨基萘的纯度。

    Process for the preparation of alkali metal diphenylates and free
hydroxydiphenyls
    6.
    发明授权
    Process for the preparation of alkali metal diphenylates and free hydroxydiphenyls 失效
    制备碱金属二苯基酯和游离羟基二苯基的方法

    公开(公告)号:US4467123A

    公开(公告)日:1984-08-21

    申请号:US459738

    申请日:1983-01-20

    CPC分类号: C07C37/04

    摘要: Hydroxydiphenyls can be prepared by reacting diphenylsulphonic acids or their alkali metal salts with an alkali metal hydroxide at elevated temperature and elevated pressure, in the presence of water. For this purpose, the diphenylsulphonic acids or their alkali metal salts are reacted, at a temperature between 280.degree. and 330.degree. C. and a pressure of up to 120 bar, with an amount of aqueous alkali metal hydroxide having a concentration of at least 50% by weight, such that, after all acidic groups have been neutralized, 3 to 25 mols of alkali metal hydroxide per equivalent of sulphonate group are present in the reaction mixture. Mineral acids are added to the alkaline reaction mixture, after it has been cooled and diluted with water, until the pH value is less than 8, and the precipitated hydroxydiphenyl is isolated at a temperature from -5.degree. C. to +100.degree. C.

    摘要翻译: 羟基二苯可以通过使二苯基磺酸或其碱金属盐与碱金属氢氧化物在高温和高压下,在水的存在下反应来制备。 为此,二苯基磺酸或其碱金属盐在280-330℃的温度和至多120巴的压力下反应,一定量的碱金属氢氧化物水溶液的浓度至少为50 重量%,使得在所有酸性基团被中和后,每当量磺酸盐基团中存在3至25摩尔碱金属氢氧化物基团。 将矿物酸加入到碱性反应混合物中,冷却并用水稀释,直到pH值小于8,沉淀的羟基二苯在-5℃至+ 100℃的温度下分离。