반응 #2469079

반응 방정식

NaH

5-fluoro-3-methyl-1H-indole

NH2OSO3H

→

5-fluoro-3-methyl-indol-1-ylamine

용매

DMF

반응 조건

후처리

1. 1
   온도the mixture is then warmed to rt
2. 2
   workup.STIRRINGstirred for 2 h
3. 3
   기타The mixture is quenched with MeOH
4. 4
   workup.ADDITIONdiluted with water
5. 5
   추출extracted with EtOAc
6. 6
   건조dried (Na2SO4)
7. 7
   여과filtered
8. 8
   농축concentrated

실험 절차

A suspension of NaH (2.01 g, 50.3 mmol, 60% in mineral oil) in DMF (45 mL) at 0° C. is treated with 5-fluoro-3-methyl-1H-indole (500 mg, 3.55 mmol), and the mixture is stirred at 0° C. for 1 h. NH2OSO3H (1.9 g, 16.75 mmol) is added portion wise, and the mixture is then warmed to rt and stirred for 2 h. The mixture is quenched with MeOH, diluted with water, extracted with EtOAc, dried (Na2SO4), filtered and concentrated to afford 5-fluoro-3-methyl-indol-1-ylamine. MS: 165 (M+H); 1H NMR (300 MHz, CD3OD): δ 2.22 (s, 3H), 6.86 (m, 1H), 6.99 (s, 1H), 7.08 (m, 1H), 7.36 (m, 1H).

출처