反应详情

NCS (38 mg, 0.288 mmol) was added to a solution of 4-amino-3-chloro-N,N-dimethylbenzamide (52 mg, 0.262 mmol) in MeCN (520 mL). The reaction mixture was refluxed for 1 hour before being concentrated under vacuum. The residue was purified via Biotage silica gel column chromatography eluting with (cyclohexane/EtOAc 80/20 to 60/40) to afford the title product as a white solid (57 mg, 93%). 1H NMR (500 MHz, CDCl3) d 3.06 (s, 6H), 4.68 (br s, 2H), 7.34 (s, 2H). LC (Method D)-MS (ESI, m/z) tR 1.50 min, 233 [(M+H+), 100%].

1. temperatureThe reaction mixture was refluxed for 1 hour
2. concentrationbefore being concentrated under vacuum
3. customThe residue was purified via Biotage silica gel column chromatography
4. washeluting with (cyclohexane/EtOAc 80/20 to 60/40)