Convenient Modular Syntheses of Fluorous Secondary Phosphines and Selected Derivatives
作者:Charlotte Emnet、Róbert Tuba、J. A. Gladysz
DOI:10.1002/adsc.200505145
日期:2005.11
Reactions of the fluorous primary phosphines Rfn(CH2)2PH2 [Rfn=(CF2)n−1CF3; n=6, 8, 10] and Rfn′CHCH2 [(n′=6, 8, 10) (1 : 1; THF, reflux) in the presence of AIBN give the title compounds [Rfn(CH2)2][Rfn′(CH2)2]PH [n/n′=6/6 (4, 55%), 8/8 (5, 58%), 10/10 (6, 53%), 8/6 (7, 52%), 10/8 (8, 51%)] as low-melting white solids on up to 10-g scales. The chiral tertiary phosphine [Rf6(CH2)2][Rf8(CH2)2][Rf10(CH2)2]P
氟伯膦的反应R fn(CH 2)2 PH 2 [R fn =(CF 2)n-1 CF 3;N = 6,8,10]和R FN' CHCH 2 [(N'= 6,8,10)(1:1; THF,回流)在AIBN的存在下,得到标题化合物[R FN(CH 2)2 ] [R FN'(CH 2)2 ] PH [N / N'= 6/6(4,55%),8/8(5,58%),10/10(6,53%),8 / 6(7,52%),10/8(8,51%)]的低熔点白色固体(最大10克刻度)。在VAZO存在下,类似地由7和R f10 CHCH 2制备手性叔膦[R f6(CH 2)2 ] [R f8(CH 2)2 ] [R f10(CH 2)2 ] P(9)(纯净,100°C; 67%)。5与THF·BH 3的反应生成膦硼烷5· BH 3(95%)。将三光气[(CCl 3 O)2 CO]添加到5或R f8(CH 2)2 PH