A kind of preparation method of alkyl tin compound or benzyl tin compound
An alkyl tin compound and compound technology, applied in the direction of tin organic compounds, etc., can solve the problems such as the inability to meet the synthesis requirements of tin reagents, the poor compatibility of reactive functional groups, etc., and achieve low cost, good tolerance and universality, and cost reduction. Effect
- Summary
- Abstract
- Description
- Claims
- Application Information
AI Technical Summary
Problems solved by technology
Method used
Image
Examples
Embodiment 1
[0036] Synthesis of Benzyltri-n-Butylstannane
[0037] Under a nitrogen atmosphere, add 55 mg (ie 0.2 mmol) of p-toluenesulfonyl hydrazone of benzaldehyde to a 10 mL elongated reaction tube, the mass fraction of 11 mg (ie 0.22 mmol, the molar ratio to hydrazone is 1.1:1) is 50% Sodium hydride, 11mg (ie 0.04mmol, the molar ratio to hydrazone is 0.2:1) of tetra-n-butylammonium chloride. Add 3 mL of anhydrous and anaerobic-treated toluene, and stir at room temperature for 10 minutes. Then add 58 mg (0.2 mmol, 54 μL, molar ratio to hydrazone: 1:1) of tri-n-butyltin hydride with a 100 μL microsampler, and react at 110 ° C for 6 h. After the reaction, use petroleum ether to elute on a short column of silica gel for filtration and rough separation, concentrate the filtrate on a rotary evaporator, and then use petroleum ether to perform column chromatography purification to obtain benzyl tri-n-butylstannane, whose structure is as follows: Shown:
[0038]
[0039] The compound is...
Embodiment 2
[0042] Synthesis of p-methylbenzyltri-n-butylstannane
[0043] Under a nitrogen atmosphere, add 58 mg (ie 0.2 mmol) of p-toluenesulfonyl hydrazone of p-toluene aldehyde to a 10 mL elongated reaction tube at a mass fraction of 11 mg (ie 0.22 mmol, the molar ratio to hydrazone is 1.1:1) 50% sodium hydride, 11mg (ie 0.04mmol, the molar ratio to hydrazone is 0.2:1) of tetra-n-butylammonium chloride. Add 3 mL of anhydrous and anaerobic-treated toluene, and stir at room temperature for 10 minutes. Then add 58 mg (0.2 mmol, 54 μL, molar ratio to hydrazone: 1:1) of tri-n-butyltin hydride with a 100 μL microsampler, and react at 110 ° C for 6 h. After the reaction, use sherwood oil to elute on a short column of silica gel for filtration and rough separation, concentrate the filtrate on a rotary evaporator, and then use sherwood oil to carry out column chromatography purification to obtain p-methylbenzyl tri-n-butylstannane, which The structure is as follows:
[0044]
[0045] The...
Embodiment 3
[0048] Synthesis of 4-tert-butylbenzyltri-n-butylstannane
[0049] Under nitrogen atmosphere, add 660mg (ie 0.2mmol) p-toluenesulfonyl hydrazone of p-tert-butylbenzaldehyde, 11mg (ie 0.22mmol, the molar ratio to hydrazone is 1.1:1) mass in a 10mL elongated reaction tube The fraction is 50% sodium hydride, 11 mg (ie 0.04 mmol, the molar ratio to hydrazone is 0.2:1) of tetra-n-butylammonium chloride. Add 3 mL of anhydrous and anaerobic-treated toluene, and stir at room temperature for 10 minutes. Then add 58 mg (0.2 mmol, 54 μL, molar ratio to hydrazone: 1:1) of tri-n-butyltin hydride with a 100 μL microsampler, and react at 110 ° C for 6 h. After the reaction, use petroleum ether to elute on a silica gel short column for filtration and rough separation, concentrate the filtrate on a rotary evaporator, and then use petroleum ether for column chromatography purification to obtain 4-tert-butylbenzyltri-n-butylstannane , whose structure is shown in the following formula:
[0050...
PUM
Login to View More Abstract
Description
Claims
Application Information
Login to View More