Reaktion #816457
ord-f86d8678885b459999024205244d1183
Reaktionsgleichung
Edukte
Reagenzien
Keine
Lösungsmittel
Reaktionsbedingungen
Temperatur
130°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.
Aufarbeitung
- 1workup.WAITat 140° C. for 1 h
- 2workup.WAITfinally at 140° C. for 1.5 h
- 3SonstigeThe mixture was purified
Vorschrift
A mixture of 2-butyl-4-chloro-5-phenylisothiazol-3(2H)-one 1,1-dioxide (300 mg, 0.90 nmol) and 1-(5-amino-1-benzofuran-2-yl)ethanone (387 mg, 2.21 mmol) in dry MeCN (4.5 mL) was heated in a microwave reactor at 130° C. for 1 h, then at 130° C. for 1 h, then at 140° C. for 1 h and finally at 140° C. for 1.5 h. The mixture was purified using preparative HPLC (Kromasil-column C8, 0.1M NH4OAc/MeCN, gradient) to give the title compound (116 mg, 28%); 1H NMR (400 MHz, CD3CN): δ 7.86 (bs, 1H), 7.34-7.32 (m, 1H), 7.26-7.22 (m, 1H), 7.03-7.15 (m, 7H), 3.76 (t, 2H), 1.78-1.87 (m, 2H) 1.43-1.54 (m, 2H), 1.05 (t, 3H); Mass Spectrum: M−H+ 437