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    • 4. 发明授权
    • Process for the manufacture of
6-methyl-3,4-dihydro-1,2,3-oxathiazin-4-one-2,2-dioxide
    • 制备6-甲基-3,4-二氢-1,2,3-氧杂噻嗪-4-酮-2,2-二氧化物的方法
    • US3968107A
    • 1976-07-06
    • US596247
    • 1975-07-16
    • Karl ClaussErwin SchmidtHartmut PietschHarald Jensen
    • Karl ClaussErwin SchmidtHartmut PietschHarald Jensen
    • A23L27/30C07D291/06
    • C07D291/06
    • 6-Methyl-3,4-dihydro-1,2,3-oxathiazin-4-one-2,2-dioxide and the nontoxic salts thereof are prepared by reacting acetoacetic acid with fluorosulfonyl isocyanate at a temperature of from -20.degree.C to +50.degree.C in the presence of from 0.5 to 2 moles, calculated on the FSI used, of an alkali methal fluoride or a tertiary amine of the formulaN(R.sub.1)(R.sub.2)(R.sub.3)in which R.sub.1, R.sub.2, R.sub.3 represent identical or different alkyl radicals having from 1 to 10 carbon atoms, two of the radicals R.sub.1 to R.sub.3 optionally form together an alkylene radical having from 4 to 5 carbon atoms which may contain N, O, or S as hetero atom, or one of the radicals R.sub.1 to R.sub.3 represents a phenyl radical, or of pyridine or quinoline, or of a mixture of the aforesaid compounds, and transforming the salt of acetoacetamide-N-sulfofluoride obtained into the oxathiazinone salt or the free oxathiazinone by a treatment with aqueous and/or alcoholic bases.
    • 6-甲基-3,4-二氢-1,2,3-氧杂噻嗪-4-酮-2,2-二氧化物及其无毒盐通过乙酰乙酸与氟磺酰基异氰酸酯在-20℃的温度下反应制备 在式(I)(R 2)(R 3)的碱金属氟化物或叔胺的存在下,在0.5〜2摩尔的存在下,在0.5〜2摩尔的存在下,将R 1,R 2,R 3 代表具有1至10个碳原子的相同或不同的烷基,基团R 1至R 3中的两个任选地可以含有具有4至5个碳原子的亚烷基,其可以含有N,O或S作为杂原子,或者 基团R 1至R 3表示苯基或吡啶或喹啉或上述化合物的混合物,并将获得的乙酰乙酰胺-N-磺酰氟盐转化为氧杂二恶嗪酮盐或游离的恶唑二酮通过用水和 /或酒精基地。
    • 8. 发明授权
    • Process for the preparation of N-vinyl-N-alkyl-carboxylic acid amides
    • 制备N-乙烯基-N-烷基 - 羧酸酰胺的方法
    • US4322271A
    • 1982-03-30
    • US149742
    • 1980-05-14
    • Harald JensenErwin SchmidtMichael MitzlaffJurgen CramerRudolf PistoriusHartmut PietschKlaus Dehmer
    • Harald JensenErwin SchmidtMichael MitzlaffJurgen CramerRudolf PistoriusHartmut PietschKlaus Dehmer
    • C07C67/00C07C231/00C07C231/08C07C231/12C07C102/00
    • C07C231/00
    • N-Vinyl-N-alkyl-carboxylic acid amides are prepared, starting from N-ethyl-carboxylic acid amides, in a 3-stage process consisting of the following stages:(a) anodic alkoxylation of the N-ethyl-carboxylic acid amides to give N-.alpha.-alkoxyethyl-carboxylic acid amides;(b) alkylation of these N-.alpha.-alkoxyethyl-carboxylic acid amides with an alkyl halide or dialkyl sulfate in an alkaline medium to give N-.alpha.-alkoxyethyl-N-alkyl-carboxylic acid amides; and(c) splitting off of alcohol from the products of stage (b) by heating to temperatures between about 60.degree. and about 350.degree. C.Instead of stages (b) and (c), it is also possible to carry out the following stages after stage (a):(b.sub.1) splitting off of alcohol from the N-.alpha.-alkoxyethylcarboxylic acid amides obtained in stage (a) by heating to temperatures of about 60.degree. to about 600.degree. C., to give N-vinyl-carboxylic acid amides; and(c.sub.1) alkylation of these N-vinyl-carboxylic acid amides by reaction with an alkylating agent of the same type as in stage (b) in an alkaline medium.The N-vinyl-N-alkyl-carboxylic acid amides obtained by the process are valuable intermediate products, in particular for the manufacture of homopolymers and copolymers with interesting properties.
    • N-乙烯基-N-烷基 - 羧酸酰胺由N-乙基 - 羧酸酰胺开始,由以下阶段组成的3阶段方法制备:(a)N-乙基 - 羧酸酰胺的阳极烷氧基化 得到N-α-烷氧基乙基 - 羧酸酰胺; (b)在碱性介质中将这些N-α-烷氧基乙基 - 羧酸酰胺与烷基卤化物或二烷基硫酸盐烷基化,得到N-α-烷氧基乙基-N-烷基 - 羧酸酰胺; 和(c)通过加热到约60℃至约350℃的温度,从阶段(b)的产物中分离出醇。代替阶段(b)和(c),还可以进行以下 阶段(a)之后的阶段:(b1)通过加热到约60℃至约600℃的温度,从阶段(a)中获得的N-α-烷氧基乙基羧酸酰胺中分离出醇,得到N-乙烯基 - 羧酸酰胺; 和(c1)通过与碱性介质中与阶段(b)相同类型的烷基化剂反应来烷基化这些N-乙烯基羧酸酰胺。 通过该方法获得的N-乙烯基-N-烷基 - 羧酸酰胺是有价值的中间产物,特别是用于制造具有有趣特性的均聚物和共聚物。