반응 #72650

ord-8825132270bb4ac48c621bba3d01d5cb

용매

반응 조건

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

후처리

  1. 1
    온도After the reaction mixture was cooled down
  2. 2
    여과the resulting precipitate was collected by filtration
  3. 3
    세척rinsed with ethanol
  4. 4
    기타dried in the air

실험 절차

A mixture of 2-chloroquinazolin-4-amine (Example 38) (100 mg, 0.56 mmol) and hydrazine (0.09 mL, 2.79 mmol) in ethanol (5 mL) was heated in a sealed tube at 80° C. overnight. After the reaction mixture was cooled down, the resulting precipitate was collected by filtration, rinsed with ethanol and dried in the air to give the title compound (84 mg, 86%). 1H NMR (400 MHz, DMSO-d6) δ4.2 (bs, 2H), 4.6 (bs, 2H), 7.0 (t, J=7.2 Hz, 1H), 7.27 (d, J=8.0 Hz, 1H), 7.43 (s, 1H), 7.61 (s, 1H), 7.87 (d, J=7.6 Hz, 1H).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US08541421B2uspto-grants-2013_09