反应详情

Piperonyl (0.06 g, 04 mmol), is added to a solution of benzo[1,3]dioxol-5-ylmethyl-(5-butyl-3-chloro-6-phenyl-pyridazin-4-ylmethyl)-amine (0.042 g, 0.1 mmol) in CH2ClCH2Cl (5 mL) and HOAc (0.5 mL). The mixture is stirred at room temperature for 45 minutes, NaBH(OAc)3 (0.127 g, 0.6 mmol) is then added and the mixture is stirred overnight. The solvent is removed in vacuo, the residue is partitioned between saturated aqueous Na44CO3 solution (20 mL) and EtOAc (20 mL), and the organic layer is washed with water (15 mL), brine (15 mL), and then dried (Na2SO4). Evaporation of the solvent a in vacuo provides the compound shown above as a yellow oil. Preparative TLC (3:1 Hexane, EtOAc) of the residue provides a light yellow oil. LC-MS (M+1) 544, 1H NMR (δ, CDCl3) 7.37-7.48 (m, 5H), 6.77 (s, 2H), 6.72 (s, 4H), 5.91 (s, 4H), 3.78 (s, 2H), 3.49 (s, 4H), 2.69 (t, J=7.2 Hz, 2H), 0.85-1.02 (m, 4H), 0.59 (t, J=7.0 Hz, 3H).

1. stirringthe mixture is stirred overnight
2. customThe solvent is removed in vacuo
3. customthe residue is partitioned between saturated aqueous Na44CO3 solution (20 mL) and EtOAc (20 mL)
4. washthe organic layer is washed with water (15 mL), brine (15 mL)
5. dry with materialdried (Na2SO4)
6. customEvaporation of the solvent a in vacuo
7. customprovides the compound