反应详情

温度

30 °C

A solution of POCl3 was slowly added to anhydrous DMF over a period of 20 minutes and the temperature was maintained around 30° C. 3′-Chloroacetophenone solution in anhydrous DMF was added to the above solution and the reaction temperature was allowed to rise to around 50° C. Hydroxylamine HCl was added to the reaction solution, portionwise, over 1 hour. A volume of 500 mL of water was added to form precipitate, stirred for 1 hour and the precipitate was collected on a Buchner funnel, washed with H2O, and dried to afford a yellow crystalline compound, mp 60-62° C. 1H NMR (DMSO-d6) δ1.60 (s, 6H), 7.30 (d, 1H, J=8.41 Hz), 7.41 (d, 1H, J=8.41 Hz), 10.47 (s, 1H); MS(+APCI)m/z 213(M+H); Anal. Calc. For C9H9ClN2O2: C, 50.84; H, 4.27; N, 13.17. Found: C, 50.99; H, 4.28; N, 12.98.

1. customto rise to around 50° C
2. customto form precipitate
3. customthe precipitate was collected on a Buchner funnel
4. washwashed with H2O
5. customdried
6. customto afford a yellow crystalline compound, mp 60-62° C