All sensitive materials were transferred under inert atmosphere conditions, using a dry box or Schlenk apparatus. Solvents were dried by reflux over Na or H2Ca in an Ar atmosphere. All starting materials were [wiki]pu[/wiki]rified by crystallization or distillation under low pressure.
General Procedure for the Titanium-Induced Couplings. TiCl3 (1.03g, 6.7 mmol) and 1.5 g of Zn-Cu coupleb were covered with 20 mL of dry solvent . The mixture was refluxed for 1 h with effective stirring under Ar atmosphere. .A solution of 3.35 mol of the carbonyl compound in 5 mL of dry solvent was added at once, and refluxing was continued for the amount of time indicated in Table I. To the reaction mixture was added 25 g of silica gel, and the solvent was removed under vacuum, the residue being incorporated at the top of a silica gel column. Stilbenes were eluted with CH2Cl2, normally giving crystalline compounds.
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最新回复
wcrxy (2008-10-03 21:05:56)
meteor_121 (2008-10-03 23:06:57)
QUOTE:
我使用灵格斯翻译家,但是有些语言组织不如天天看化学的来的顺,就来问问wenkine (2008-10-03 23:58:16)
[wiki]钛[/wiki]诱导结合反应的常规过程
三[wiki]氯[/wiki]化钛(1.03克,6.7毫摩尔)和1.5克[wiki]锌[/wiki]铜合金加入20毫升干燥溶剂浸没,混合物在氩气保护中搅拌回流1小时,立即加入3.35摩尔的羰基化合物(用5ml干燥溶剂溶解),继续回流,回流时间见表1。反应混合物加入25克[wiki]硅[/wiki]胶,减压蒸除溶剂,剩余物置硅胶柱顶部,用二氯[wiki]甲烷[/wiki]洗脱1,2-二[wiki]苯[/wiki]乙烯,正常得到结晶化合物。
meteor_121 (2008-10-04 01:33:49)
QUOTE:
非常感谢,呵呵