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小木虫7718

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Ylidene 3 and elemental sulfur (1.2 atom equiv) are suspended in tetrahydrofuran (10 mL/g 3) and warmed to an  internal temperature of 35 C. A solution of sodium
bicarbonate (1.0 equiv in 5 mL of water/g 3) is added over~1 h. The mixture is stirred at 35 C for approximately 30 min before the solution is transferred to a separatory funnel and washed with 12.5% aqueous NaCl and 25% aqueous
NaCl. The products 4 were isolated by crystallization.
关键是不晓得碳酸氢钠的量应该加多少,硫该加多少。化合物3用量为1.68g(10mmol).

[ Last edited by 小木虫7718 on 2010-8-3 at 16:15 ]
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xiaoboshen

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小木虫7718(金币+20, 翻译EPI+1):谢谢了 2010-08-03 19:02:39
将亚基3和元素硫分散在10 mL/g 3的四氢呋喃溶液中,加热使内部温度达到35度。然后加入碳酸氢钠溶液。将混合物在35度下搅拌大约30min,之后再将混合物转移到一分液漏斗中,用12.5%的氯化钠水溶液和25%的氯化钠水溶液进行洗涤。通过结晶分离得到产品4。
亚基3:硫=1:1.2
碳酸氢钠:5mL 水中含1.0g碳酸氢钠
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2楼2010-08-03 16:31:54
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