The doubly base-stabilized diborane(4) (HB(μ-hpp))2 (hpp = 1,3,4,6,7,8-hexahydro-2H-pyrimido[1,2-a]pyrimidinate): synthesis by catalytic dehydrogenation and reactions with S8 and disulfides
In this work we report on new experiments on the catalytic dehydrogenation of [H2B(μ-hpp)]2 leading to the doubly base-stabilized diborane(4) [HB(μ-hpp)]2 featuring two hpp bridges (hpp = 1,3,4,6,7,8-hexahydro-2H-pyrimido[1,2-a]pyrimidinate) under mild conditions. Several dehydrogenation (pre)cataly...
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| Main Authors: | , , , , |
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| Format: | Article (Journal) |
| Language: | English |
| Published: |
August 24, 2010
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| In: |
European journal of inorganic chemistry
Year: 2010, Issue: 33, Pages: 5201-5210 |
| ISSN: | 1099-0682 |
| DOI: | 10.1002/ejic.201000637 |
| Online Access: | Resolving-System, lizenzpflichtig, Volltext: https://doi.org/10.1002/ejic.201000637 Verlag, lizenzpflichtig, Volltext: https://onlinelibrary.wiley.com/doi/abs/10.1002/ejic.201000637 |
| Author Notes: | Nikola Schulenberg, Oxana Ciobanu, Elisabeth Kaifer, Hubert Wadepohl, and Hans-Jörg Himmel |
| Summary: | In this work we report on new experiments on the catalytic dehydrogenation of [H2B(μ-hpp)]2 leading to the doubly base-stabilized diborane(4) [HB(μ-hpp)]2 featuring two hpp bridges (hpp = 1,3,4,6,7,8-hexahydro-2H-pyrimido[1,2-a]pyrimidinate) under mild conditions. Several dehydrogenation (pre)catalysts were tested. The best one turned out to be Ru3(CO)12, allowing quantitative dehydrogenation already at 60 °C. Subsequently we subjected [HB(μ-hpp)]2 to reactions with S8 and disulfides (Ph2S2 and Bn2S2, Bn = benzyl). Reaction with S8 leads to oxidative insertion of one sulfur atom into the B-B bond and formation of [HB(μ-hpp)]2(μ-S). In the case of disulfides, substitution reactions leading to the doubly base-stabilized diborane(4) species [RSB(μ-hpp)]2 and HB(μ-hpp)2BSR (R = Ph or Bn) compete with sulfuration again leading to [HB(μ-hpp)]2(μ-S). |
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| Item Description: | Im Titel erscheinen die Bezeichnungen "HB(μ-hpp)" und "1,2-a" in eckigen Klammern Beim Ausdruck [HB(μ-hpp)]2 erscheint die Ziffer 2 tiefgestellt Beim Ausdruck S8 erscheint die Ziffer 8 tiefgestellt Gesehen am 04.07.2023 |
| Physical Description: | Online Resource |
| ISSN: | 1099-0682 |
| DOI: | 10.1002/ejic.201000637 |