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【答案】应助回帖
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ringzhu(金币+1): 多谢交流~~ 2011-06-05 12:10:57
lgq101(金币+10, 翻译EPI+1): 谢谢~~~ 2011-06-05 21:44:12
General Procedure for Evans Butadiene [4 + 2 + 2] Cycloaddition (7).
合成Evans Butadiene [4 + 2 + 2] Cycloaddition (7)的一般实验步骤。
Vacuum-dried resin 3 (800 mg, 0.86 meq, 1.0 eq) was swollen with CH2Cl2 (20 mL) for 10 min, then cooled to 0 °C.
真空干燥过的树脂3(800 mg, 0.86 meq, 1.0 eq)在20毫升的二氯甲烷中溶解10分钟之后降温到0度，
Solid m-CPBA (580 mg, 2.58 mmol, 3.0 eq) was added and the reaction was stirred at 0 °C for 1 h, then allowed to warm to RT and stirred for 6 h.
固体m-CPBA (580 mg, 2.58 mmol, 3.0 eq)在0度加入到上述反应液中，继续搅拌1个小时，再升到室温搅拌6个小时，
The resin was washed and dried, then swollen with toluene (20mL) for 10min。
反应液洗涤，干燥，再次溶解在20毫升的甲苯中，10分钟之后，
A stock solution of Rh(IMes)(COD)Cl4, where IMes is 1,3-bis(2,4,6-trimethylphenyl)imidazoly-2-ylidene, and AgOTf (1∶2 molar ratio, 0.1 M Rh in degassed toluene, 3.44 mL, 0.34 mmol Rh, 0.4 eq) was added to the resin,
将准备好的Rh(IMes)(COD)Cl4和AgOTf (1∶2 molar ratio, 0.1 M Rh in degassed toluene, 3.44 mL, 0.34 mmol Rh, 0.4 eq)加到反应中，其中IMes是指1,3-bis(2,4,6-trimethylphenyl)imidazoly-2-ylidene
and the reaction atmosphere was flushed with 1,3-butadiene gas, then the mixture was stirred under a balloon of 1,3-butadiene at RT for 2 h, refilling the balloon when empty.
向气球中充满1,3-butadiene，并置换反应体系中的气体，当气球空了，重新充满，在室温下反应2小时之后，
The balloon was removed and the mixture was heated to 108 °C for 24 h. The resin was cooled, washed, and dried to afford cyclooctapyrrolidines 7.
将气球取走，反应加热到108度反应24小时，降温，洗涤，干燥，得到了cyclooctapyrrolidines 7。 |
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