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    Preparation of alkyl 5-oxo-6-heptenoates, and novel intermediate for the preparation thereof
    1.
    发明授权
    Preparation of alkyl 5-oxo-6-heptenoates, and novel intermediate for the preparation thereof 失效
    5-氧代-6-庚烯酸烷基酯的制备及其制备的新型中间体

    公开(公告)号：US5659070A

    公开(公告)日：1997-08-19

    申请号：US595051

    申请日：1996-02-01

    申请人： Klaus Ebel ,  Matthias Eiermann ,  Thomas Papkalla

    发明人： Klaus Ebel ,  Matthias Eiermann ,  Thomas Papkalla

    IPC分类号： C07C67/333 ,  C07C69/738 ,  C07C69/73

    CPC分类号： C07C69/738 ,  C07C67/333

    摘要： A process for preparing alkyl 5-oxo-6-heptenoates of the formula I ##STR1## where X and Y are hydrogen or methyl, and R.sup.1 is C.sub.1 -C.sub.8 -alkyl, byA) reacting 5-acetyl-2-norbornene with a dialkyl carbonate [CO(OR.sup.2).sub.2, where R.sup.2 is C.sub.1 -C.sub.4 -alkyl,] in the presence of a base to give an alkyl 3-(2-norbornen-5-yl)-3-oxopropionate II,B) reacting the ester II on the presence of a base with an unsaturated compound of the formula III ##STR2## where Z is CN or CO.sub.2 R.sup.3, where R.sup.3 is C.sub.1 -C.sub.4 -alkyl, and hydrolyzing the product of the reaction of compound II with compound III to a 5-(2-norbornen-5-yl)-5-oxopentanoic acid of the formula IV,C) esterifying the acid IV to give a 5-(2-norbornen-5-yl)-5-oxopentanoic ester of the formula V, andD) converting the ester V by thermal cleavage into an alkyl 5-oxo-6-heptenoate I. The invention also relates to intermediates for preparing the esters I, to the use thereof and to an improved process for preparing alkyl 3-(2-norbornen-5-yl)-3-oxopropionates.

    摘要翻译： 制备式I的烷基5-氧代-6-庚烯酸酯的方法，其中X和Y是氢或甲基，R 1是C 1 -C 8烷基，A）使5-乙酰基-2- 降冰片烯与碳酸二烷基酯[CO（OR 2）2，其中R 2是C 1 -C 4 - 烷基）]在碱的存在下反应，得到3-（2-降冰片烯-5-基）-3-氧代丙酸烷基酯II，B ）在碱存在下使酯II与式III的不饱和化合物（III）反应，其中Z是CN或CO 2 R 3，其中R 3是C 1 -C 4烷基，并水解化合物的反应产物 II化合物与式IV的5-（2-降冰片烯-5-基）-5-氧代戊酸反应，C）酯化酸IV，得到5-（2-降冰片烯-5-基）-5- 式V的氧代戊酸酯，和D）通过热裂解将酯V转化为5-氧代-6-庚烯酸酯I。本发明还涉及制备酯I的中间体及其改进方法 用于制备3-（2-降冰片烯-5-基）-3-氧代丙酸烷基酯。

    Preparation of methane sulfonic acid
    3.
    发明授权
    Preparation of methane sulfonic acid 失效
    甲磺酸的制备

    公开(公告)号：US06207025B1

    公开(公告)日：2001-03-27

    申请号：US09269759

    申请日：1999-04-08

    申请人： Matthias Eiermann ,  Thomas Papkalla

    发明人： Matthias Eiermann ,  Thomas Papkalla

    IPC分类号： C07C30300

    CPC分类号： C07C303/14 ,  C07C309/04

    摘要： A process for preparing methanesulfonic acid by irradiating a mixture comprising acetic acid, sulfur dioxide and oxygen with light, wherein the reaction mixture is irradiated with an average cumulative irradiance in the range from 240 to 320 mm of from 0.05 to 50 mmol quanta/cm2h at the light entry area.

    摘要翻译： 通过用光照射包含乙酸，二氧化硫和氧气的混合物来制备甲磺酸的方法，其中反应混合物在240至320mm范围内的平均累积辐照度为0.05至50mmol量子/ cm 2h， 光入口区域。