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lgq101

木虫 (小有名气)

[求助] 求一段有机合成翻译~~~谢谢

General Procedure for Sulfinamide N-Alkylation (3, 4). Propargyl sulfonamide resin 2 (800 mg, 0.92 meq, 1.0 eq) was swollen with THF (20 mL) for 10 min, then the mixture was cooled to −78 °C and a solution of n-BuLi (2.4 M in hexanes, 2.02 mmol, 2.2 eq) was added by syringe. The reaction was stirred for 45 min, then hexamethylphosphoramide (640 μL, 3.68 mmol, 4.0 eq) was added. After stirring for an additional 30 min, allyl or propargyl bromide (9.2 mmol, 10 eq) was added. The mixture was stirred at −78 °C for 6 h, then allowed to warm to RT overnight. The reaction was quenched with water (100 mL), then the resin was washed and dried to afford enynes 3 or diynes 4.
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hongliannu

木虫 (小有名气)

【答案】应助回帖

★
爱与雨下(金币+1): 欢迎常来~! 2011-08-21 11:47:10
lgq101(金币+9, 翻译EPI+1): 谢谢~~~~~ 2011-08-22 09:30:15
亚磺酰胺的N-烷基化的基本过程。用四氢呋喃(20ml)溶胀炔丙基磺胺树脂2(800mg,0.92当量,1.0eq)10分钟,然后混合物冷却到-78℃再用注射器加入正丁基锂溶液(浓度2.4M,正己烷为溶剂,2.02mmol,2.2当量)。反应搅拌45分钟,然后加入六甲基磷酰三胺(640ul,3.68mmol,4.0当量)。再搅拌30分钟后,再加入丙烯基或炔丙基溴化物(9.2mmol,10当量)。混合物在-78℃搅拌6小时,然后一整夜升温到室温。使用100ml水终止反应,然后洗涤、干燥树脂后得到烯炔3或diynes4.
2楼2011-08-21 11:33:42
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liubencai

木虫之王 (文坛精英)

【答案】应助回帖

★ ★
爱与雨下(金币+1): 欢迎常来~! 2011-08-21 11:47:34
sltmac(金币+1): 2011-08-22 07:14:35
lgq101(金币+11): 谢谢~~~~~ 2011-08-22 09:30:24
合成N -烷基(3,4)亚磺酰胺的通用步骤。炔丙基磺酰胺树脂2(800毫克,0.92毫当量,1.0当量)用四氢呋喃(20毫升)溶胀10分钟,然后将混合物冷却至-78°C,再用注射器加入n-丁基锂(2.4 M正己烷溶液,2.02毫摩尔,2.2当量)溶液。反应并搅拌45分钟,然后加入六甲基磷酰胺(640μL,3.68毫摩尔,4.0当量)。再搅拌30分钟后,加入烯丙基或炔丙基溴(9.2毫摩尔,10当量)。在-78°C搅拌混合物6小时,然后保暖至室温过夜。加水(100毫升)使反应停止,然后洗涤树脂,干燥得到烯炔3或二炔4。
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3楼2011-08-21 11:41:12
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