Borane-triethylamine complex synthesis
- Product Name:Borane-triethylamine complex
- CAS Number:1722-26-5
- Molecular formula:C6H18BN
- Molecular Weight:115.02
16940-66-2
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1722-26-5
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Yield:1722-26-5 98 %Spectr.
Reaction Conditions:
Stage #1:sodium tetrahydroborate with sodium hydroxide in water for 24 h;Inert atmosphere;
Stage #2:triethylamine hydrochloride;triethylamine in toluene at 22 - 40;
Steps:
Synthetic Sodium Borohydride Dihydrate with 100 mL Toluene and Solid NEt3HClA three-neck flask containing a solids addition funnel, thermometer and a nitrogen gas purge was charged with 10 grams of SBH AF Grans, 10 grams of water and 0.1 grams of NaOH. The slurry was stirred for 24 hours until a solid mass formed. Then 100 mL of anhydrous toluene and 30 mL of NEt3 were added. This slurry was stirred and 1 equivalent of solid NEt3HCl (36.2 g) was added so that the temperature of the reaction did not increase above 40° C.A large amount of gas evolved when the temperature of the reaction rose above 30° C. After 6 hours, 60 mL of water were added to dissolve all of the solids in the reaction pot. The resulting two-phase solution was placed into a separatory funnel and the bottom phase was washed with 3×100 mL of fresh toluene. All of the toluene phases were combined. Both the toluene and water phases were analyzed by 1H and 11B NMR.Spectroscopic data for NEt3BH3. 11B NMR (tol d8), δ-30.8 ppm, (q, JB-H=98.3 Hz, 1B). 1H (tol d8) δ=2.32 ppm (q, j1-3=7.2 Hz, 6H) δ 0.84 ppm, (t, JH-H=7.3 Hz, 9H) Material Amount Total amount charged Amount charged recovered recovered SBH AF Grans 10.0 g Water 10.0 gNEt3 25 g Toluene 100 mL (86.5 g) 123.76 gNEt3HCl 36.2 g Water added 60 mL (60 g) 87.88 g Toluene wash 1 100 mL (86.5 g) 56.5 g Toluene wash 2 100 mL (86.5 g) 70.50 g Toluene wash 3 100 mL (86.5 g) 100.27 g 383.03 g Yield 98%
References:
Cartolano, Anthony Rocco;Ivanov, Sergei Vladimirovich;Teich, Cheryl Irene;Yamamoto, John Hiroshi US2010/130780, 2010, A1 Location in patent:Page/Page column 2; 5
16940-66-2
8 suppliers
$19.19/100ml
121-44-8
823 suppliers
$9.00/5g
1722-26-5
149 suppliers
$23.30/5G
16940-66-2
8 suppliers
$19.19/100ml
1722-26-5
149 suppliers
$23.30/5G
121-43-7
343 suppliers
$13.00/25mL
121-44-8
823 suppliers
$9.00/5g
1722-26-5
149 suppliers
$23.30/5G
1095-03-0
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1333-74-0
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121-44-8
823 suppliers
$9.00/5g
1722-26-5
149 suppliers
$23.30/5G