반응 #1563948

반응 방정식

7-fluoro-5-nitro-2,3-dihydrobenzo[b][1,4]dioxine

→

7-fluoro-2,3-dihydrobenzo[b][1,4]dioxin-5-amine

용매

methanol

반응 조건

후처리

1. 1
   여과The reaction mixture was filtered over celite bed
2. 2
   세척washed with methanol
3. 3
   농축The filtrate and the washings were concentrated under reduced pressure

실험 절차

10% Pd/C (400 mg) was added to a solution of 7-fluoro-5-nitro-2,3-dihydrobenzo[b][1,4]dioxine (2.0 g, 10 mmol) in methanol (50 mL) and stirring was continued at 25° C. under H2 atmosphere for 3 h. The reaction mixture was filtered over celite bed and washed with methanol. The filtrate and the washings were concentrated under reduced pressure to afford 7-fluoro-2,3-dihydrobenzo[b][1,4]dioxin-5-amine (Int-52) as pale brown liquid. MS (ESI): m/z 170.1 (M+H).

출처