반응 #45665

반응 방정식

tert-butylchlorodiphenylsilane

N-methylethanolamine

imidazole

→

compound

수율 39.0%

[2-(tert-Butyldiphenylsiloxy)ethyl]methylamine

수율 39.0%

용매

N,N-dimethylformamide

N,N-dimethylformamide

반응 조건

후처리

1. 1
   기타The solvent was evaporated away under reduced pressure
2. 2
   workup.DISSOLUTIONthe residue was dissolved in ethyl acetate
3. 3
   세척the solution was washed with saturated sodium hydrogencarbonate water, water and saturated brine
4. 4
   건조Next, the organic layer was dried over anhydrous magnesium sulfate
5. 5
   여과filtered
6. 6
   농축the filtrate was concentrated under reduced pressure

실험 절차

Under nitrogen atmosphere, an N,N-dimethylformamide (33 ml) solution of tert-butylchlorodiphenylsilane (8.78 g, 32.0 mmol) was dropwise added at room temperature to an N,N-dimethylformamide (100 ml) solution of N-methylethanolamine (2.00 g, 26.6 mmol) and imidazole (2.72 g, 39.9 mmol), and stirred for 5.5 hours. The solvent was evaporated away under reduced pressure, then the residue was dissolved in ethyl acetate, and the solution was washed with saturated sodium hydrogencarbonate water, water and saturated brine. Next, the organic layer was dried over anhydrous magnesium sulfate, filtered, and the filtrate was concentrated under reduced pressure. The resulting residue was subjected to silica gel column chromatography, and the eluate with ethyl acetate gave the entitled compound (3.21 g, 39%) as a pale yellow oil.

출처