Synthesis of alkali metal substituted borohydride reagents
A technology of borohydride and alkali metal, which is used in the synthesis field of replacing borohydride reagents, and can solve problems such as danger, intractability, and high temperature
- Summary
- Abstract
- Description
- Claims
- Application Information
AI Technical Summary
Problems solved by technology
Method used
Examples
Embodiment 1
[0061] Example 1: Potassium tri-sec-butyl borohydride in THF (two steps, single reactor)
[0062] 13.7 grams of metallic potassium, 241.7 grams of dry tetrahydrofuran, and 1.0 grams of phenanthrene were added to a Parr pressure reactor equipped with a back pressure regulator (set at 95 psig) and a bubbler system. The mixture was heated to about 65°C to melt the potassium metal, and then stirred to disperse the potassium metal in tetrahydrofuran. The temperature was then increased to 85°C.
[0063]Hydrogen pressure is applied to the reactor until the reactor pressure reaches 50 psig. The pressure is maintained for about 8 hours. The reactor was then cooled to 25°C and depressurized. Then 65.4 g of tri-sec-butylborane was added to keep the reaction temperature below 30°C. After the addition of tri-sec-butylborane, the reaction mixture was stirred for about 1 hour, and then filtered through a filter. The filtrate contains potassium tri-sec-butyl borohydride. The yield is almost quant...
Embodiment 2
[0064] Example 2: Potassium tri-sec-butyl borohydride in THF (two steps, single reactor)
[0065] 23.46 grams of metallic potassium, 136.64 grams of dry tetrahydrofuran and 1.71 grams of phenanthrene were added to a Parr pressure reactor equipped with a back pressure regulator (set at 95 psig) and a bubbling system. The mixture was heated to about 65°C to melt the potassium metal, and then stirred to disperse the potassium metal in tetrahydrofuran. Then the temperature was increased to 85°C.
[0066] Hydrogen pressure is applied to the reactor until the reactor pressure reaches 50 psig. The pressure is maintained for about 8 hours. The reactor was then cooled to 25°C and depressurized. Then, 111.48 grams of tri-sec-butylborane was added to keep the reaction temperature below 30°C. After the addition of tri-sec-butylborane, the reaction mixture was stirred for about 1 hour, and then filtered through a filter. The filtrate contains potassium tri-sec-butyl borohydride. The yield is a...
Embodiment 3
[0067] Example 3: Potassium tri-sec-butyl borohydride in THF (one step, single reactor)
[0068] 16.4 grams of metallic potassium, 265.0 grams of dry tetrahydrofuran and 64.4 grams of tri-sec-butylborane were added to a Parr pressure reactor equipped with a back pressure regulator (set at 95 psig) and a bubbling system. The mixture was heated to about 65°C to melt the potassium metal, and then stirred to disperse the potassium metal in tetrahydrofuran. Then the temperature was increased to 85°C.
[0069] Hydrogen pressure is applied to the reactor until the reactor pressure reaches 50 psig. The pressure is maintained overnight. The reactor was then cooled to 25°C and depressurized. Then filter the contents of the reactor with a filter. The filtrate contains potassium tri-sec-butyl borohydride. The yield was 95%.
PUM
Login to View More Abstract
Description
Claims
Application Information
Login to View More