Addition of 1 equiv of water to Mo(CAr_p)(OR_F9)₃ (Ar_p = p-methoxyphenyl; OR_F9 = OC(CF₃)₃) in the presence of 5% NEt₃ (vs Mo) in THF led to the formation of Mo(O)(CHAr_p)(OR_F9)₂(THF)₂ in good yield. Mo(O)(CHAr_p)(OR_F9)₂(THF)₂ reacts with 2 equiv of LiOHMT (OHMT = O-2,6-mesityl₂C₆H₃) at room temperature to yield Mo(O)(CHAr_p)(OHMT)₂ and with 2 equiv of NaOTPP (OTPP = 2,3,5,6-tetraphenylphenoxide) to yield Mo(O)(CHAr_p)(OTPP)₂. In the presence of TMEDA (2.5 equiv), Mo(CR)(OR_F9)₃ (R = Ar_p, mesityl, or t-Bu) reacts with 1 equiv of water to yield Mo(O)(CHR)(OR_F9)₂(TMEDA) complexes, from which (when R = t-Bu) TMEDA is readily displaced by 2,2′-bipyridyl to give Mo(O)(CH-t-Bu)(OR_F9)₂(bipy). Mo(O)(CH-t-Bu)(OR_F9)₂(bipy) was converted into Mo(O)(CH-t-Bu)Cl₂(bipy) readily, from which Mo(O)(CH-t-Bu)Cl(OHMT)(3-Brpy) (3-Brpy = 3-bromopyridine) and Mo(O)(CH-t-Bu)Cl(OHIPT)(3-Brpy) (OHIPT = O-2,6-(2,4,6-i-Pr₃C₆H₂)₂C₆H₃) were prepared. X-ray studies were carried out on Mo(O)(CHAr_p)(OR_F9)₂(THF)₂, Mo(O)(CH-t-Bu)(OR_F9)₂(TMEDA), Mo(O)(CHAr_p)(OTPP)₂, Mo(O)(CH-t-Bu)Cl(OHMT)(3-Brpy), and Mo(O)(CH-t-Bu)Cl(OHIPT)(3-Brpy).

中文翻译：

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通过将水加至炔烃炔配合物中来合成“无磷”钼氧代炔烃配合物

在THF中在5％NEt ₃（vs Mo）存在下，向Mo（CAr _p）（OR _F9）₃（Ar _p =对甲氧基苯基； OR _F9 = OC（CF ₃）₃）中添加1当量水以良好的产率形成Mo（O）（CHAr _p）（OR _F9）₂（THF）₂。Mo（O）（CHAr _p）（OR _F9）₂（THF）₂与2当量的LiOHMT反应（OHMT = O -2,6-甲磺酸₂ C ₆ H ₃）在室温下生成Mo（O）（CHAr _p）（OHMT）₂和2当量的NaOTPP（OTPP = 2,3,5,6-四苯酚）生成Mo（O）（CHAr _p）（OTPP）₂。在TMEDA（2.5当量）存在的情况下，Mo（CR）（OR _F9）₃（R = Ar _p，1,3,4-叔丁基）与1当量的水反应生成Mo（O）（CHR）（OR _F9）₂（TMEDA）配合物，从中（当R = t -Bu时）TMEDA容易被2,2'-联吡啶取代，得到Mo（O）（CH- t- Bu）（OR _F9）₂（bipy）。Mo（O）（CH- t -Bu）（OR _F9）₂（bipy）容易地转化为Mo（O）（CH- t- Bu）Cl ₂（bipy），从中Mo（O）（CH- t- Bu）Cl（OHMT）（3-Brpy）（3- Brpy = 3-溴吡啶）和Mo（O）（CH- t -Bu）Cl（OHIPT）（3-Brpy）（OHIPT = O -2,6-（2,4,6- i -Pr ₃ C ₆ H ₂）制备₂ C ₆ H ₃）。对Mo（O）（CHAr _p）（OR _F9）₂（THF）₂，Mo（O）（CH- t- Bu）（OR _F9）₂（TMEDA），Mo（O）进行X射线研究（CHAR _p（OTPP）₂，Mo（O）（CH- t- Bu）Cl（OHMT）（3-Brpy）和Mo（O）（CH- t- Bu）Cl（OHIPT）（3-Brpy）。