CAS: 18166-02-4; (Trimethylsilyl)Methanamine

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📜氯甲基三甲基硅烷置于ammonium Hydroxide,Sodium Hydroxide体系中,用 甲醇,乙醚 用作溶剂,115.0 °C,2.07 Mpa 条件下,反应 16.0H,以48%的收率获得氨甲基三甲基硅烷
参考文献:分批和连续流一锅法使用胺重氮化生成甲硅烷基化的重氮试剂.
标题:分批和连续流一锅法使用胺重氮化生成甲硅烷基化的重氮试剂.
摘要:报道了使用间歇和连续流合成通过三甲基甲硅烷基甲胺(tmsch 2 Nh 2)的重氮化而新颖地合成三甲基甲硅烷基重氮甲烷(tmschn 2).后者每天可生产275克(2.4摩尔)tmschn 2.在开发的反应条件下,其他甲硅烷基化的甲胺也成功地进行了反应,以提供各种含硅的重氮甲烷试剂.通过公开间歇和连续流一锅酯化和1,3-偶极环加成方法,突出了该方法的适用性.此外,公开了在连续流动中羧酸与甲硅烷基化和取代的甲胺的高产率酯化.最后,报道了用于制备tmschn 2的2-Methf溶液的后处理和纯化程序,该溶液可用于铑催化的亚甲基化和同源化反应.
Doi:10.1002/anie.201612235

专利信息

专利号:US-4914233-A
优先权日:1988-03-01
标题:Synthesis of beta-thymidine
发明人：FRESKOS JOHN N; SENARATNE K PUSHPANANDA A
权利人:ETHYL CORP
摘要:A process is provided in which a mixture of alpha- and beta-anomers is converted selectively to the desired beta-thymidine. The process involves the following steps: (a) converting a mixture of alpha- and beta-anomers of tetra-O-acylribofuranose to tri-O-acyl-β-ribothymidine; (b) converting tri-O-acyl-β-ribothymidine to β-ribothymidine; (c) converting β-ribothymidine to 2,2'-anhydro-β-thymidine; (d) converting 2,2'-anhydro-β-thymidine to 2'-halo-2'-deoxy-5-methyluridine; and (e) converting 2'-halo-2'-deoxy-5-methyluridine to beta-thymidine. The mixture of alpha- and beta-anomers of tetra-O-acylribofuranose may be produced by any suitable procedure such as by converting lower alkyl ribofuranoside to the tetra-O-acylribofuranose mixture. The lower alkyl ribofuranosides may in turn be produced by various methods. However, a desirable way of effecting this conversion involves use of D-ribose as the starting material which is converted to the lower alkyl ribofuranoside.