英语翻译ExperimentalSectionAmixtureof1b(1.0mmol,226mg),DLP(1.0mmol,398mg),anddimethylphosphite(5mmol,550mg)incyclohexane(10mL)washeatedat808Cfor6h.Aftercompletion(monitoringbyGC),thesolutionwascooledandthecyclohex

Question

英语翻译
Experimental Section
A mixture of 1b (1.0 mmol,226 mg),DLP (1.0 mmol,398 mg),and
dimethyl phosphite (5 mmol,550 mg) in cyclohexane (10 mL) was
heated at 808C for 6 h.After completion (monitoring by GC),the
solution was cooled and the cyclohexane evaporated under reduced
pressure.CH3CN (10 mL) was added to precipitate the by-products
derived from DLP.After filtration and evaporation,the residue was
purified by flash chromatography (EtOAc/cyclohexane,80:20) to
afford the phosphonate 2b (306 mg,91%).
Received:April 14,2005
Published online:July 20,2005
.Keywords:alkynes · cyclopentanes · fused-ring systems ·
hydrogen transfer · radical reactions
Table 1:Dimethyl phosphite mediated hydrogen abstraction [cyclization
according to Eq.(4)].
Entry Substrate Product d.r.[a] Yield [%][b]
R Y Z
1 1b H Me Me 2b – 91
2 1c iPr CO2Et H 2c 82:18 91
3 1d H Ph H 2d 92:8 55
4 1e H OTBS H 2e 73:27 79
[a] Determined by GC or NMRanalysis of the crude reaction mixture.
[b] Yield of isolated product.TBS=tert-butyldimethylsilyl.
Communications
5274

Answer 1

实验性部分 混合物1b (1.0 mmol,226 毫克),DLP (1.0 mmol,398 毫克),和 二甲基亚磷酸盐(5 mmol,550 毫克) 在环己烷里(10 机器语言) 是 加热在808C 为6 h .在完成(监视以后由GC),解答冷却了并且环己烷被蒸发了在减少之下 压力.CH3CN (10 机器语言) 增加沉淀副产物 从DLP 获得.在滤清和蒸发以后,残滓是 由一刹那色谱法(EtOAc/cyclohexane,80:20) 净化 买得起phosphonate 2b (306 毫克,91%) .接受:2005 年4月14 日 在网上出版:2005 年7月20 日 Keywords:炔.cyclopentanes .熔化圆环系统.氢调动.根本反应 表1:二甲基亚磷酸盐斡旋了氢抽象[ 环合 根据Eq .(4) ] .词条基体产品d.r.[a ] 出产量[ %][b ] R Y Z 1 1b H 我我2b - 91 2 1.c iPr CO2.Et H 2c 82:18 91 3 1d H 酸碱度H 第2 92:8 55 4 1e H OTBS H 2.e 73:27 79 [ a ] 由粗暴反应混合物的GC 或NMRanalysis 确定.[ b ] 出产量被隔绝的产品.TBS=tert-butyldimethylsilyl .通信 5274
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