HRID1922412

反应详情

EQUATION

反应方程式

HRID 1922412 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Phenyl methyl(2-(6-nitro-2-oxo-3,4-dihydroquinolin-1(2H)-yl)ethyl)carbamate (1.29 g, 3.49 mmol) was dissolved by stirring in ethanol (40 mL) and THF (30 mL) in a round bottom flask. The solution was stirred under an atmosphere of hydrogen for 6 h at room temperature. When TLC confirmed the reaction was completed, the mixture was filtered through celite, and the filtrate was concentrated. The resulting residue was chromatographed on silica gel eluting with ethyl acetate, giving a white/pink foam. Yield: 990 mg, 84%. 1H NMR (DMSO-d6) δ 7.36 (m, 2H), 7.20 (m, 1H), 7.01 (m, 2H); 6.91 (d, 1H, J=8.4 Hz), 6.43 (m, 2H), 4.87 (s, 2H), 4.11 and 4.03 (2m, 2H), 3.56 and 3.44 (2t, 2H, J=6.0 Hz), 2.99 and 2.87 (2s, 3H), 2.66 (m, 2H), 2.43 (m, 2H); ESI-MS (m/z, %): 362 (MNa+, 35), 340 (MH+, 100), 202 (44).

WORKUP

后处理

  1. filtrationthe mixture was filtered through celite
  2. concentrationthe filtrate was concentrated
  3. customThe resulting residue was chromatographed on silica gel eluting with ethyl acetate
  4. customgiving a white/pink foam