반응 #85747

반응 방정식

dioxane

(R)-2-methyl-N—((S)-1-(4-(trifluoromethoxy)phenyl)ethyl)propane-2-sulfinamide

ether

→

(S)-1-(4-(trifluoromethoxy)phenyl)ethanamine

수율 80.5%

용매

HCl

반응 조건

후처리

1. 1
   기타the resulting cloudy solution sonicated for 1 min, upon which time the white solid product
2. 2
   기타precipitates out
3. 3
   여과The solid was filtered through a Buchner funnel
4. 4
   세척washed 5 times with ˜20 ml ether
5. 5
   기타to air dry

실험 절차

(R)-2-methyl-N—((S)-1-(4-(trifluoromethoxy)phenyl)ethyl)propane-2-sulfinamide (5.08 g, 16.4 mmol) was dissolved by swirling in 4M HCl in dioxane (16.4 ml, 65.6 mmol), at room temperature. The solution was allowed to sit for 1 hr with occasional swirling. To the clear solution was added 45 ml ether and the resulting cloudy solution sonicated for 1 min, upon which time the white solid product precipitates out. The solid was filtered through a Buchner funnel, washed 5 times with ˜20 ml ether and allowed to air dry. Obtained (S)-1-(4-(trifluoromethoxy)phenyl)ethanamine (3.2 g, 13.2 mmol, 80% yield), 1H NMR (400 MHz, CD3OD) δ 1.64 (d, J=6.90 Hz, 3H) 4.52 (q, J=6.88 Hz, 1H) 7.38 (d, J=8.02 Hz, 2H) 7.57 (d, J=8.71 Hz, 2H). LCMS m/z 206.1 (M+H)+, Rt 0.52 min.

출처