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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
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
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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