期刊文献+

(E)-叔丁基(1-碘基-1-戊烯基-3-氧代)二甲基硅烷的合成 被引量:1

A Aacile Synthesis of(E)-tert-butyl(1-iodopent-1-en-3-yloxy)-dimethylsilane
下载PDF
导出
摘要 以(R)苯甲基环氧丙醇((S)环氧丙醇苄基化作用得到)为原料,经格氏反应、TBS羟基保护、脱苄基、缩合、碘仿反应,其中,考察了格氏反应的萃灭方法,萃取溶剂的选择:饱和氯化氨溶液萃灭,二乙醚作为萃取溶剂。也考察了TBS羟基保护反应中的溶剂筛选:采用二氯甲烷作为溶剂,产物收率较高。同时讨论了超低温缩合反应体系中,氮气保护是体系确保收率的关键控制点,最后分析合成化合物f中影响收率关键点:催化剂的用量和滴加化合物e的四氢呋喃溶液温度(2℃)。经过以上合成步骤,得到目标产物,总收率为28.25%,产物结构经过1H NMR确证,合成路线尚未见文献报道。 (R) benzyl epoxy propyl alcohol (S) epoxy propyl alcohol benzylation get) as raw material, the grignard reaction, TBS hydroxy protection, to take off the benzyl, condensation, and iodoform reaction, the extract out method of grignard reaction was inspected. The extraction solvent conditions were saturated solution of ammonia chloride extraction out and diethyl ether as extraction solvent. Also inspected the TBS hydroxy protective reaction solvent in the screening, u- sing dichloromethane as solvent, the product yield was quite high. At the same time, the ultra -low temperature condensation reaction system was discussed, nitrogen protection was a system ensured to yield the key point, in the final analysis, and synthetic compounds affect yield key points were the dosage of catalyst and drop and compound e tetrahydrofuran solution temperature (2 ℃). Through above synthetic process, the target product was got, and the overall yield was 28.25%, the product structure by1H NMR confirmed, synthetic route was not reported in the literature to see.
作者 王胜 李宁东
出处 《广州化工》 CAS 2013年第4期113-115,共3页 GuangZhou Chemical Industry
关键词 (R)苯甲基环氧丙醇 TBS羟基保护 碘仿 合成 (R) benzyl epoxy propyl alcohol TBS hydroxy protection iodoform synthesis
  • 相关文献

参考文献6

  • 1Baker, Raymond, Castro, Jose L. From Journal of the Chemical Socie-ty, Perkin Transactions 1 : Organic and Bio - Organic Chemistry (1972-1999), 1990(l):47-65.
  • 2Petasis, Nicos A. From U. S. Pat. Appl. Publ.,20090291916, 26,Nov 2009.
  • 3Kitano, Yasunori, et al. From Tetrahedron Letters, 1987 , 28 ( 50):6351 -6354.
  • 4Cossy, Janine, et al. From European Journal of Organic Chemistry,2001(2):339 -348.
  • 5Du, Xiangwei, et al. From Chemistry - - A European Journal, 2008,14(31):9495-9498.
  • 6Petasis, Nicos A. From U. S* Pat. Appl. Publ. , 20050228047, 13Oct2005.

同被引文献630

  • 1李静,高中良,刘英浪,郭湘立.双(4-氟苯基)氯甲基甲基硅烷的合成[J].河北工业大学学报,2013,42(2):46-48. 被引量:2
  • 2武江红,杜志平,台秀梅,赵永红,王天壮.乙烯基三(β-甲氧基乙氧基)硅烷原位改性纳米SiO_2的制备与表征[J].中国粉体技术,2013,19(4):5-9. 被引量:3
  • 3谢凯明,王斌,朱春华.巯基改性有机硅防水剂的制备与应用[J].乙醛醋酸化工,2013(3):10-13. 被引量:3
  • 4浙江新安化工集团股份有限公司.浙江新安化工集团股份有限公司2013年年度报告[EB/OL].(2014-04-22)[2014-05-05].http://file.finance.sina.com.cn/211.154.219.97:9494/MRGG/CNSESH-STOCK/2014/2014-4/2014-04-22/1371264.PDF.
  • 5蓝星化工新材料股份有限公司.蓝星化工新材料股份有限公司2013年年度报告[EB/OL].(2014-04-16)[2014-04-20].http://file.finance.sina.com.cn/211.154.219.97:9494/MRGG/CNSESH-STOCK/2014/2014-4/2014-04-16/1362604.
  • 6东岳集团有限公司.东岳集团有限公司2013年年报[EB/OL].http://www.dongyuechem.corn/UploadFiles/2014-3/News/201432021261919002.pdf,(2014-03-20)[2014-04-20].
  • 7唐山三友化工股份有限公司.唐山三友化工股份有限公司2013年年度报告及摘要(修订版)[EB/OL].(2014-04-01)2014-04-20].http://vip.stock.finance.sina.com.cn/corp/view/vCB-AllBulle-tinDetail.php?stockid=sh600409&id=1343316.
  • 8江苏宏达新材料股份有限公司.江苏宏达新材料股份有限公司2013年年度报告[EB/OL].(2014-04-26)[2013-05-05].http://file.finance.sina.com.cn/211.154.219.97:9494/MRGG/CNSESZ-STOCK/2014/2014-4/2014-04-26/1388067.PDF.
  • 9成都硅宝科技股份有限公司.成都硅宝科技股份有限公司2013年年度报告[EB/OL].http://vip.stock.finance.sina.com.cn/corp/view/vCB-AllBulletinDetail.php?gather=1&id=1310016,(2014-03-07)[2014-04-20].
  • 10湖北回天胶业股份有限公司.湖北回天胶业股份有限公司2013年度报告[EB/OL].(2014-03-26)[2014-04-20].http://vip.stock.finance.si-na.com.cn/corp/view/vCB-AllBulletin.php?stockid=300041&Page=2.

引证文献1

二级引证文献2

相关作者

内容加载中请稍等...

相关机构

内容加载中请稍等...

相关主题

内容加载中请稍等...

浏览历史

内容加载中请稍等...
;
使用帮助 返回顶部