반응 #80143

ord-0dfa46575f2b49228650894a4566bd8b

반응 조건

온도
80°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    여과The mixture was then filtered
  2. 2
    농축the filtrate concentrated in vacuo

실험 절차

To a stirred solution of 100 mg (01.17 mmol) (2-benzoylamino-4-methoxy-benzothiazol-7-yl)-(4-methyl-benzyl)-carbamic acid 2,2,2-trichloro-ethyl ester in 3 ml acetic acid at room temperature was added 90 mg (1.34 mmol) activated zinc powder and the mixture was heated at 80° C. for 16 hours. The mixture was then filtered and the filtrate concentrated in vacuo. Flash chromatography (ethyl acetate/hexane) afforded 15 mg (21%) N-[4-methoxy-7-(4-methyl-benzylamino)-benzothiazol-2-yl]-benzamide as a yellow crystalline solid, ES-MS m/e (%): 426 (M+Na+, 27), 404 (M+H+, 100), and 10 mg (13%) N-{7-[acetyl-(4-methyl-benzyl)-amino]-4-methoxy-benzothiazol-2-yl}-benzamide as a yellow crystalline solid, ES-MS m/e (%): 468 (M+Na+, 12), 446 (M+H+, 100).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US06713499B2uspto-grants-2004_03