Silane Deuteration Catalyzed by Ruthenium Bis(dihydrogen) Complexes or Simple Metal Salts
作者:Katharine A. Smart、Emmanuelle Mothes-Martin、Tatsuro Annaka、Mary Grellier、Sylviane Sabo-Etienne
DOI:10.1002/adsc.201300902
日期:2014.3.10
The deuteration of a diverse group of silanes: alkyl‐, aryl‐, alkoxy‐ and chlorosilanes, siloxane and silazane, under an atmosphere of dideuterium (D2) was explored with ruthenium bis(dihydrogen) dihydride complexes and hydrated metal salts. Deuterium incorporation of greater than 97% for the silanes O(SiMe2H)2, Et3SiH, (EtO)3SiH and Me2ClSiH was possible with 0.1 mol% of the ruthenium complex [RuH2(η2‐H2)2(PCyp3)2]
在双氘(D 2)气氛下,用二氢化钌(二氢)配合物和水合金属盐探索了多种硅烷的氘化:烷基硅烷,芳基硅烷,烷氧基硅烷和氯硅烷,硅氧烷和硅氮烷。用于硅烷O(森达的大于97%的氘掺入2 2H)2,等3的SiH,(ETO)3的SiH和Me 2 ClSiH是可能的,0.1%(摩尔)钌络合物的[期RuH 2(η 2 -H 2)2(PCyp 3)2 ] [对于O(SiMe 2 H)2为0.05摩尔%]在纯硅烷中于30°C和1 bar D 2的条件下进行3.5 h催化时。的空气稳定的三氯化钌盐的RuCl 3 ⋅xħ 2 O的也代表O的氘化(森达的有效催化剂2 2H)2和Et 3 SiH基; 为93%和90%的两种硅烷的氘掺入分别是可能的相同的条件下,作为[期RuH 2(η 2 -H 2)2(PCyp 3)2 ]用0.1%催化剂载量。三氯化铑(RhCl )催化O(SiMe 2 H)2的氢-氘交换3 ⋅xħ 2