초록 ▼

Disclosed is a method for the preparation of decaborane-14(B10H14) in high yields from B5H9 which involve three basic procedure steps as follows: (1) conversion of B5H9 to a solid, [N(CH3)4][B9H14], by reacting NaH in a tetrahydrofuran (THF) solution in the presence of [N(CH3)4][Cl]; (2) performing

Disclosed is a method for the preparation of decaborane-14(B10H14) in high yields from B5H9 which involve three basic procedure steps as follows: (1) conversion of B5H9 to a solid, [N(CH3)4][B9H14], by reacting NaH in a tetrahydrofuran (THF) solution in the presence of [N(CH3)4][Cl]; (2) performing a hydride abstraction on the solid after removal of THF by reacting, while stirring, a boron trihalide selected from BBr3 and BCl3 to form B10H14; and, (3) separating the B10H14 from the solid reaction mixture by a sublimation procedure.

대표청구항 ▼

A method for the preparation of decaborane-14(B10H14) through the conversion of B5H9 to [N(CH3)4][B9H14], the hydride ion abstraction reaction of [N(CH3)4][B9H14], by a boron trihalide to form B10H14, and the separation and recovery of B10H14, in pure form by a sublimation process, said method compr

A method for the preparation of decaborane-14(B10H14) through the conversion of B5H9 to [N(CH3)4][B9H14], the hydride ion abstraction reaction of [N(CH3)4][B9H14], by a boron trihalide to form B10H14, and the separation and recovery of B10H14, in pure form by a sublimation process, said method comprising completing steps (i-IX) as set forth hereinbelow and relating to said conversion, completing steps (X-XIII) as set forth hereinbelow and relating to said hydride ion abstraction reaction, and completing steps (XIV-XV) as set forth hereinbelow and relating to said separation and recovery as follows: (i) adding to a first reaction vessel provided with a means for stirring and while maintained in a dry box of N2 atmosphere, a predetermined weight of NaH and [(CH3)4N][Cl]to provide a 1:1 molar ratio of said NaH and said [(CH3)4N][Cl]; (ii) removing said first reaction vessel from said dry box and attaching said first reaction vessel to a vacuum means for removing of dry box N2; (iii) condensing a predetermined volume of dry tetrahydrofuran into said first reaction vessel maintained at about -78°C. while condensing of said dry tetrahydrofuran into said first reaction vessel to form a reaction mixture; (iv) subjecting said first reaction vessel and said reaction mixture to a liquid N2 Dewar container for cooling prior to condensing a predetermined volume of B5H9 measured at 0°C. into said reaction mixture, said predetermined volume of said B5H9 providing a 2 molar ratio of said B5H9 to said 1:1 molar ratio of said NaH and [N(CH3)4][Cl]; (v) warming said first reaction vessel and said reaction mixture to a room temperature of about 26°C.-27°C. and stirring said reaction mixture vigorously for about 12 hours to complete a reaction period to form the solid reaction products [N(CH3)4][B9H14]and NaCl in said reaction mixture; (vi) cooling said first reaction vessel and said solid reaction products to -196°C. and removing hydrogen and other volatiles; (vii) warming said first reaction vessel and said solid reaction products to about 0°C. while removing said solvent under vacuum from said solid reaction products [N(CH3)4][B9H14]and NaCl; (viii) transferring said solid reaction products to a second reaction vessel in a dry box, said second reaction vessel having a smaller capacity than said first reaction vessel; (ix) removing said second reaction vessel from dry box and evacuating said second reaction vessel of dry box N2; (x) condensing a predetermined molar volume of a boron trihalide selected from BCl3 freed from HCl or BBr3 freed from HBr into said second reaction vessel maintained at -196°C., said predetermined molar volume of said boron trihalide being in ratio of 1:2 to said condensed B5H9; (xi) warming contents of said second reaction vessel to about 11°C. to room temperature and reacting while stirring said contents of said second reaction vessel for a predetermined time period of about 4 hours to form reaction products including B10H14 by hydride ion abstraction; (xii) cooling said second reaction vessel and said reaction products including B10H14 and removing hydrogen; (xiii) warming said second reaction vessel to a room temperature range of about 26°C.-27°C. and removing trace of volatile products by vacuum pumping; (xiv) transferring said second reaction vessel to a dry box; and, (xv) separating said B10H14 by sublimation from said second reaction vessel and recovering said B10H14 in pure form.