반응 #86484

반응 방정식

ether water

DIEA

2-(methylamino)ethanol

tert-butylchlorodimethylsilane

→

title compound

수율 56.0%

2-((tert-butyldimethylsilyl)oxy)-N-methylethanamine

수율 56.0%

용매

DCM

반응 조건

후처리

1. 1
   workup.ADDITIONwas added
2. 2
   추출The aqueous layer was extracted with ether three times
3. 3
   건조The combined organic layer was dried over MgSO4
4. 4
   기타evaporated
5. 5
   기타was dried under high vacuum

실험 절차

2-(methylamino)ethanol (1.0 g, 13.3 mmol) was stirred in DCM (25.0 ml) under atmosphere of nitrogen. DIEA (3.23 ml, 18.6 mmol) followed by tert-butylchlorodimethylsilane (2.0 g, 13.3 mmol) was added and the reaction mixture was stirred at room temperature over night. The reaction mixture was poured into ether/water. The aqueous layer was extracted with ether three times. The combined organic layer was dried over MgSO4 and evaporated and remaining material was dried under high vacuum to afford title compound (1.4 g, yield: 56%). 1H-NMR (400 MHz, CDCl3) δ 0.08 (s, 6H) 0.91 (s, 9H) 1.93 (br. s., 1H) 2.48 (s, 3H) 2.71 (t, 2H) 3.75 (t, 2H).

출처