Process for the production of 1,3,4-thiadiazol-5(4H)-onyl
dithiophosphoric acid esters
    4.
    发明授权
    Process for the production of 1,3,4-thiadiazol-5(4H)-onyl dithiophosphoric acid esters 失效
    制备1,3,4-噻二唑-5(4H) - 基二硫代磷酸酯的方法

    公开(公告)号:US4035378A

    公开(公告)日:1977-07-12

    申请号:US627998

    申请日:1975-11-03

    摘要: 1,3,4-Thiadiazol-5-(4H)-onyl-(4)-methyl dithiophosphoric acid ester of the formula ##STR1## wherein each of R, R.sub.1 and R.sub.2 methyl or ethyl and Y represents oxygen or sulphur, are prepared by condensing a thiophosphate acid of the formula ##STR2## or an alkali metal or ammonium salt thereof, with a 1,3,4-thiadiazole of the formula ##STR3## with formaldehyde in an aqueous medium consisting essentially of 60-98 wt % of sulphuric acid, the amount of sulphuric acid is at least 0.7 mol per mol of free thiophosphoric acid, if free acid is used, and 1.7 mol per mol of thiophosphoric acid salt, if a salt is used. The temperature of the reaction mixture is maintained at 15.degree.-60.degree. C. The process is particularly useful in the preparation of O,O-dimethyl-S-[2-methoxy-1,3,4-thiadiazol-5(4H)-onyl-(4)-methyl]-dithiophosphate (methidathion).

    摘要翻译: 式(I)的1,3,4-噻二唑-5-(4H) - 基 - (4) - 甲基二硫代磷酸酯,其中R,R 1和R 2中的每一个是甲基或乙基,Y代表氧或硫 是通过将下式(IMAGE)的硫代磷酸或其碱金属或铵盐与式(III)的1,3,4-噻二唑与基本上由 60-98重量%的硫酸,如果使用游离酸,硫酸的量相对于每摩尔游离硫代磷酸为至少0.7摩尔,如果使用盐,硫酸的量为1.7摩尔/摩尔硫代磷酸盐。 反应混合物的温度保持在15°-60℃。该方法特别可用于制备O,O-二甲基-S- [2-甲氧基-1,3,4-噻二唑-5(4H) (4) - 甲基] - 磷酸碘(甲硫氨酸)。

    Process for the production of amino-I-acid
    5.
    发明授权
    Process for the production of amino-I-acid 失效
    制备氨基-1-酸的方法

    公开(公告)号:US4199529A

    公开(公告)日:1980-04-22

    申请号:US947291

    申请日:1978-09-29

    CPC分类号: C07C303/06

    摘要: A process for the production of amino-I-acid (2-naphthylamino-5,7-disulfonic acid) starting from Tobias acid (2-naphthylamine-1-sulfonic acid), which comprises sulfonating Tobias acid with fuming sulfuric acid (oleum) isothermically at room temperature, further sulfonating the resulting 2-naphthylamine-1,5-disulfonic acid without isolation, by rapidly heating the reaction mixture to 110.degree. to 140.degree. C. to give 2-naphthylamine-1,5,7-trisulfonic acid, hydrolyzing the trisulfonic acid in sulfuric acid having a concentration between 80 and 98%, at a temperature of 100.degree.-180.degree. C., to give the amino-I-acid, precipitating this latter from dilute sulfuric acid and isolating it from the reaction mixture, and the amino-I-acid obtained by this process.

    摘要翻译: 由Tobias酸(2-萘胺-1-磺酸)制备氨基-1-酸(2-萘基氨基-5,7-二磺酸)的方法,其包括用发烟硫酸(发烟硫酸)磺化Tobias酸, 在室温下等温,不经分离进一步磺化所得的2-萘胺-1,5-二磺酸,通过将反应混合物快速加热至110-140℃,得到2-萘胺-1,5,7-三磺酸 ,在100-180℃的温度下将浓度为80-98%的硫酸中的三磺酸水解,得到氨基-1-酸,将其从稀硫酸中沉淀出来并将其从 反应混合物和通过该方法获得的氨基-1-酸。

    Process for the production of 2-amino-1-naphthalenesulfonic acid
    6.
    发明授权
    Process for the production of 2-amino-1-naphthalenesulfonic acid 失效
    2-氨基-1-萘磺酸的制备方法

    公开(公告)号:US4510100A

    公开(公告)日:1985-04-09

    申请号:US559149

    申请日:1983-12-07

    CPC分类号: C07C309/00

    摘要: The invention relates to an improved process for the production of 2-amino-1-naphthalenesulfonic acid (Tobias acid). This improved process makes it possible to obtain Tobias acid which has only a very low content of 2-aminonaphthalene and in high space-time yield. The process starts from 2-hydroxynaphthalene and comprises the following main reaction steps:(a) the sulfonation of 2-hydroxynaphthalene to 2-hydroxynaphthalene-1-sulfonic acid (oxy-Tobias acid) with chlorosulfonic acid, in an inert organic solvent;(b) the neutralization of the liberated hydrochloric acid and excess chlorosulfonic acid still present in the reaction medium and conversion of the 2-hydroxynaphthalene-1-sulfonic acid obtained into the corresponding ammonium salt with ammonia;(c) conversion of the 2-hydroxy group into the 2-amino group by the Bucherer reaction; and(d) the subsequent precipitation of the Tobias acid with dilute sulfuric acid.

    摘要翻译: 本发明涉及一种生产2-氨基-1-萘磺酸(托比亚酸)的改进方法。 这种改进的方法使得可以获得仅具有非常低的2-氨基萘含量和高空时收率的托比亚酸。 该方法从2-羟基萘开始,包括以下主要反应步骤:(a)在惰性有机溶剂中用氯磺酸将2-羟基萘磺化为2-羟基萘-1-磺酸(氧 - 托比酸); (b)中和反应介质中仍然存在的游离的盐酸和过量的氯磺酸,并将得到的2-羟基萘-1-磺酸转化为相应的铵盐与氨; (c)通过Bucherer反应将2-羟基转化为2-氨基; 和(d)随后用稀硫酸沉淀托比亚酸。