Rhodium
(Chief Bee)
11-17-02 18:04
No 380497
      Catalytic hydrogenation at STP with Ni(OAc)2-NaBH4
(Rated as: excellent)
 Bookmark   

The addition of sodium borohydride to an aqueous solution of Nickel(II)Acetate forms a precipitate of Nickel Boride (Ni2B, P-1 Nickel) which is at least as active as Raney Nickel for catalytic hydrogenation at 1 atm.

Catalytic Hydrogenation. V. The Reaction of Sodium Borohydride with Aqueous Nickel Salts.
P-1 Nickel Boride, a Convenient, Highly Active Nickel Hydrogenation Catalyst

Charles Allan Brown
J. Org. Chem. 56, 1900-1904 (1970) (../rhodium/pdf /nickel.boride.cat-hyd-1atm.pdf)

Abstract
The reaction of sodium borohydride with aqueous solutions of nickel salts immediately produces a finely divided black precipitate. This material (P-1 nickel) is a highly active catalyst for atmospheric pressure hydrogenations, more active than Raney nickel. The hydrogenations of a variety of alkenes have been examined and all but the most hindered double bonds were reduced successfully. Certain dienes were reduced cleanly to single olefinic products. P-1 nickel has marked advantages over Raney nickel: it is not pyrophoric; it is readily prepared in situ; it is highly reproducible.
 
 
 
 
    Barium
(Hive Bee)
11-18-02 15:07
No 380674
      Chem. Rev. 1986, 86, 763-780 Synthetically useful
(Rated as: excellent)
 Bookmark   

Synthetically useful reactions with metal boride and aluminide catalysts
Chem. Rev. 86, 763-780 (1986) (../rhodium/pdf /metal.boride.review.pdf)

This paper covers:
  • The making of P1- and P2-Ni2B
  • Hydrogenation of alkenes and alkynes
  • Reduction of arenes
  • Reduction of halides
  • Reduction of nitriles
  • Reduction of nitro compounds
  • Reduction of other nitrogenous functional groups such as oximes, amides, azoxy and nitroso
  • Deoxygenation reactions
  • Desulfurization
 
 
 
 
    Rhodium
(Chief Bee)
11-18-02 19:29
No 380780
      Ref uploaded  Bookmark   

Great! I have uploaded that one to my page and linked it from your post.
 
 
 
 
    Barium
(Hive Bee)
11-19-02 17:24
No 381219
      Hmm  Bookmark   

I made som P1-Ni2B today just to see how active it was with a couple of my standard hydrogen donors.

with aq. sodium hypophosphite - very active at room temp
with MeOH/sodium hypophosphite - very active at room temp
with aq ammonium formate - active at room temp, very active at 50C
with MeOH/ammonium formate - active at room temp, very active at 50C

Now it is time to reduce something

Catalytic hydrogenation freak
 
 
 
 
    Sunlight
(Pioneer Researcher)
11-19-02 22:59
No 381312
      Nice Barium  Bookmark   

Perhaps we could check it in the CTH reductive amination. Could you detail the preparation of the catalyst ?
 
 
 
 
    Rhodium
(Chief Bee)
11-20-02 00:23
No 381352
      The preparation is available in the first post in ...  Bookmark   

The preparation is available in the first post in this thread.
 
 
 
 
    Sunlight
(Pioneer Researcher)
11-20-02 15:01
No 381573
      Ok  Bookmark   

So stupid... I have NiCl2, and there's something about bad effects of Cl and Na ions in the catalyst, it's a complication.
 
 
 
 
    Aurelius
(Hive Bee)
11-21-02 22:14
No 381939
      Example  Bookmark   

hey Barium, could you put a write up on your procedure for the reduction of (your choice) a compound including catalyst prep? 
 
 
 
 
    Rhodium
(Chief Bee)
11-21-02 22:18
No 381941
      He's done that before, just perform a search on ...  Bookmark   

He's done that before, just perform a search on his name.
 
 
 
 
    Aurelius
(Hive Bee)
11-22-02 00:42
No 381971
      Thank  Bookmark   

must have missed it