反应详情

温度

80 °C

N-[(3-Chloro-pyrazin-2-yl)-(2-phenyl-quinolin-7-yl)-methyl]-acetamide (273.0 mg, 0.702 mmol) was dissolved in 20 mL of POCl3. The reaction was heated to 80° C. for 24 h. The excess POCl3 was removed in vacuo. The residue was worked up by basifying with cold 2.0 M NH3 in IPA followed by the addition of CH2Cl2 and water. The aqueous layer was washed with CH2Cl2 (2×). The organic layers where combined, dried over sodium sulfate, filtered and concentrated in vacuo to yield a light brown oil; 1H NMR (400 MHz, CDCl3) δ 2.77 (s, 3H), 7.41-7.59 (m, 4H), 7.70-7.72 (m, 1H), 7.88-7.93 (m, 3H), 8.19-8.28 (brm, 3H), 8.55 (brs, 1H); MS (ES+): 370.96 (M+1), 372.97 (M+3), 373.98 (M+4).

1. customThe excess POCl3 was removed in vacuo
2. additionfollowed by the addition of CH2Cl2 and water
3. washThe aqueous layer was washed with CH2Cl2 (2×)
4. dry with materialdried over sodium sulfate
5. filtrationfiltered
6. concentrationconcentrated in vacuo
7. customto yield a light brown oil