反応 #79033

ord-09d31b4d213a4d988ad7af9ee4764255

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    ろ過The crystalline product was filtered
  2. 2
    その他dried (0.52 g, 69%)

実験手順

A solution of 6-(5-diethoxymethyl-furan-3-yl)-4,4-dimethyl-1,4-dihydro-benzo[d][1,3]oxazin-2-one (1.1 g, 3 mmol) was stirred in THF (20 mL) and 2N HCl (2 mL) for 1 hour. The crystalline product was filtered and dried (0.52 g, 69%): mp 262-263° C; 1H NMR (DMSO-d6) δ 10.3 (s, 1H), 9.65(s, 1H), 8.59 (s, 1H), 8.04 (s, 1H), 7.65-7.64 (d, 1H, J=1.5 Hz), 7.61-7.60 (d, 1H, J=1.8 Hz), 7.59-7.58 (d, 1H, J=1.8 Hz), 6.94-6.91 (d, 1H, J=8.2 Hz), 1.65 (s, 6H). MS (ESI) m/z 270 [M−H]−.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US06713478B2uspto-grants-2004_03