Trimethylsilylation of hemimorphite

Kazuyuki Kuroda, Chuzo Kato

    Research output: Contribution to journalArticle

    8 Citations (Scopus)

    Abstract

    Trimethylsilyl derivatives were prepared from hemimorphite by the reaction between the mineral and the trimethylsilylating reagent which was the reaction mixture of hexamethyldisiloxane, chlorotrimethylsilane and an organic solvent (the direct method of trimethylsilylation of silicates). The silylated derivatives were analyzed by gas chromatography and the gas chromatographic patterns varied with the kind of organic solvents used in the trimethylsilylating reagent. The fully silylated derivative of disilicic acid, [(CH3)3Si]6Si2O7, was obtained in a high selectivity when acetone or tetrahydrofuran was used, whereas incompletely trimethylsilylated products occurred in a high yield when an alcohol was used as the silylating reagent. A combined gas chromatography-mass spectrometric analysis of the incompletely silylated derivatives indicated that unsilylated silanol groups were esterified with an alcohol. The trimethylsilylated products obtained from hemimorphite by the Lentz method, whose trimethylsilylating reagent was the reaction mixture of hexamethyldisiloxane, hydrochloric acid, water and an organic solvent, contained incompletely trimethylsilylated derivatives even in the reaction system containing acetone or tetrahydrofuran. These incompletely silylated derivatives were considered to be the silanol-containing partial trimethylsilyl derivatives of disilicic acid on the basis of the GC-MS data.

    Original languageEnglish
    Pages (from-to)947-951
    Number of pages5
    JournalJournal of Inorganic and Nuclear Chemistry
    Volume41
    Issue number7
    DOIs
    Publication statusPublished - 1979

    Fingerprint

    reagents
    Derivatives
    gas chromatography
    tetrahydrofuran
    acetone
    alcohols
    Organic solvents
    acids
    Acetone
    hydrochloric acid
    Gas chromatography
    products
    Alcohols
    silicates
    selectivity
    minerals
    Silicates
    Acids
    Hydrochloric Acid
    Hydrochloric acid

    Cite this

    Trimethylsilylation of hemimorphite. / Kuroda, Kazuyuki; Kato, Chuzo.

    In: Journal of Inorganic and Nuclear Chemistry, Vol. 41, No. 7, 1979, p. 947-951.

    Research output: Contribution to journalArticle

    @article{d0f94da7aa2549a1a186690ff71c4925,
    title = "Trimethylsilylation of hemimorphite",
    abstract = "Trimethylsilyl derivatives were prepared from hemimorphite by the reaction between the mineral and the trimethylsilylating reagent which was the reaction mixture of hexamethyldisiloxane, chlorotrimethylsilane and an organic solvent (the direct method of trimethylsilylation of silicates). The silylated derivatives were analyzed by gas chromatography and the gas chromatographic patterns varied with the kind of organic solvents used in the trimethylsilylating reagent. The fully silylated derivative of disilicic acid, [(CH3)3Si]6Si2O7, was obtained in a high selectivity when acetone or tetrahydrofuran was used, whereas incompletely trimethylsilylated products occurred in a high yield when an alcohol was used as the silylating reagent. A combined gas chromatography-mass spectrometric analysis of the incompletely silylated derivatives indicated that unsilylated silanol groups were esterified with an alcohol. The trimethylsilylated products obtained from hemimorphite by the Lentz method, whose trimethylsilylating reagent was the reaction mixture of hexamethyldisiloxane, hydrochloric acid, water and an organic solvent, contained incompletely trimethylsilylated derivatives even in the reaction system containing acetone or tetrahydrofuran. These incompletely silylated derivatives were considered to be the silanol-containing partial trimethylsilyl derivatives of disilicic acid on the basis of the GC-MS data.",
    author = "Kazuyuki Kuroda and Chuzo Kato",
    year = "1979",
    doi = "10.1016/0022-1902(79)80068-8",
    language = "English",
    volume = "41",
    pages = "947--951",
    journal = "Polyhedron",
    issn = "0277-5387",
    publisher = "Elsevier Limited",
    number = "7",

    }

    TY - JOUR

    T1 - Trimethylsilylation of hemimorphite

    AU - Kuroda, Kazuyuki

    AU - Kato, Chuzo

    PY - 1979

    Y1 - 1979

    N2 - Trimethylsilyl derivatives were prepared from hemimorphite by the reaction between the mineral and the trimethylsilylating reagent which was the reaction mixture of hexamethyldisiloxane, chlorotrimethylsilane and an organic solvent (the direct method of trimethylsilylation of silicates). The silylated derivatives were analyzed by gas chromatography and the gas chromatographic patterns varied with the kind of organic solvents used in the trimethylsilylating reagent. The fully silylated derivative of disilicic acid, [(CH3)3Si]6Si2O7, was obtained in a high selectivity when acetone or tetrahydrofuran was used, whereas incompletely trimethylsilylated products occurred in a high yield when an alcohol was used as the silylating reagent. A combined gas chromatography-mass spectrometric analysis of the incompletely silylated derivatives indicated that unsilylated silanol groups were esterified with an alcohol. The trimethylsilylated products obtained from hemimorphite by the Lentz method, whose trimethylsilylating reagent was the reaction mixture of hexamethyldisiloxane, hydrochloric acid, water and an organic solvent, contained incompletely trimethylsilylated derivatives even in the reaction system containing acetone or tetrahydrofuran. These incompletely silylated derivatives were considered to be the silanol-containing partial trimethylsilyl derivatives of disilicic acid on the basis of the GC-MS data.

    AB - Trimethylsilyl derivatives were prepared from hemimorphite by the reaction between the mineral and the trimethylsilylating reagent which was the reaction mixture of hexamethyldisiloxane, chlorotrimethylsilane and an organic solvent (the direct method of trimethylsilylation of silicates). The silylated derivatives were analyzed by gas chromatography and the gas chromatographic patterns varied with the kind of organic solvents used in the trimethylsilylating reagent. The fully silylated derivative of disilicic acid, [(CH3)3Si]6Si2O7, was obtained in a high selectivity when acetone or tetrahydrofuran was used, whereas incompletely trimethylsilylated products occurred in a high yield when an alcohol was used as the silylating reagent. A combined gas chromatography-mass spectrometric analysis of the incompletely silylated derivatives indicated that unsilylated silanol groups were esterified with an alcohol. The trimethylsilylated products obtained from hemimorphite by the Lentz method, whose trimethylsilylating reagent was the reaction mixture of hexamethyldisiloxane, hydrochloric acid, water and an organic solvent, contained incompletely trimethylsilylated derivatives even in the reaction system containing acetone or tetrahydrofuran. These incompletely silylated derivatives were considered to be the silanol-containing partial trimethylsilyl derivatives of disilicic acid on the basis of the GC-MS data.

    UR - http://www.scopus.com/inward/record.url?scp=49249150066&partnerID=8YFLogxK

    UR - http://www.scopus.com/inward/citedby.url?scp=49249150066&partnerID=8YFLogxK

    U2 - 10.1016/0022-1902(79)80068-8

    DO - 10.1016/0022-1902(79)80068-8

    M3 - Article

    AN - SCOPUS:49249150066

    VL - 41

    SP - 947

    EP - 951

    JO - Polyhedron

    JF - Polyhedron

    SN - 0277-5387

    IS - 7

    ER -