3-PHENOXYPROPIONYL CHLORIDE

反应条件: temp:0.00; pressure:0.00; stir:

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: Phenoxypropionyl chloride (9.23 g, 0.05 mol) is dissolved in 100 ml acetone and cooled with an ice bath as sodium azide (3.6 g, 0.055 mol) in 10 ml water is added dropwise. After addition is completed, the reaction mixture is warmed to room temperature and stirred for 30 minutes. The solution is decanted and concentrated. The residue is dissolved in 100 ml ether and washed with saturated sodium bicarbonate and brine. The organic phase is separated, dried (MgSO4) and concentrated to give 6.52 g (68.0% yield) of phenoxypropionyl azide as a yellow oil which solidifies on cooling. IR (KBr) cm-1 : 2137 (N3), 1718 (C=O); 1H nmr (CDCl3) δ: 7.31 (m, 2H, phenyl H), 6.98 (t, 1H, J=7.5 Hz, phenyl H), 6.92 (m, 2H, phenyl H), 4.26 (t, 3H, J=6.3 Hz, CH2O), 2.84 (t, 3H, J=6.3 Hz, CH2C=O); 13C nmr (CDCl3) δ: 178.0, 159.0, 129.5(2C), 121.2, 114.7(2C), 62.9, 36.9. is added dropwise After addition The solution is decanted concentrated The residue is dissolved in 100 ml ether washed with saturated sodium bicarbonate and brine The organic phase is separated dried (MgSO4) concentrated

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: Phenoxypropionyl chloride (9.23 g, 0.05 mol) is dissolved in 100 ml acetone and cooled with an ice bath as sodium azide (3.6 g, 0.055 mol) in 10 ml water is added dropwise. After addition is completed, the reaction mixture is warmed to room temperature and stirred for 30 minutes. The solution is decanted and concentrated. The residue is dissolved in 100 ml ether and washed with saturated sodium bicarbonate and brine. The organic phase is separated, dried (MgSO4) and concentrated to give 6.52 g (68.0% yield) of phenoxypropionyl azide as a yellow oil which solidifies on cooling. IR (KBr) cm-1 : 2137 (N3), 1718 (C=O); 1H nmr (CDCl3) δ: 7.31 (m, 2H, phenyl H), 6.98 (t, 1H, J=7.5 Hz, phenyl H), 6.92 (m, 2H, phenyl H), 4.26 (t, 3H, J=6.3 Hz, CH2O), 2.84 (t, 3H, J=6.3 Hz, CH2C=O); 13C nmr (CDCl3) δ: 178.0, 159.0, 129.5(2C), 121.2, 114.7(2C), 62.9, 36.9. is added dropwise After addition The solution is decanted concentrated The residue is dissolved in 100 ml ether washed with saturated sodium bicarbonate and brine The organic phase is separated dried (MgSO4) concentrated

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: Phenoxypropionyl chloride (9.23 g, 0.05 mol) is dissolved in 100 ml acetone and cooled with an ice bath as sodium azide (3.6 g, 0.055 mol) in 10 ml water is added dropwise. After addition is completed, the reaction mixture is warmed to room temperature and stirred for 30 minutes. The solution is decanted and concentrated. The residue is dissolved in 100 ml ether and washed with saturated sodium bicarbonate and brine. The organic phase is separated, dried (MgSO4) and concentrated to give 6.52 g (68.0% yield) of phenoxypropionyl azide as a yellow oil which solidifies on cooling. IR (KBr) cm-1 : 2137 (N3), 1718 (C=O); 1H nmr (CDCl3) δ: 7.31 (m, 2H, phenyl H), 6.98 (t, 1H, J=7.5 Hz, phenyl H), 6.92 (m, 2H, phenyl H), 4.26 (t, 3H, J=6.3 Hz, CH2O), 2.84 (t, 3H, J=6.3 Hz, CH2C=O); 13C nmr (CDCl3) δ: 178.0, 159.0, 129.5(2C), 121.2, 114.7(2C), 62.9, 36.9. is added dropwise After addition The solution is decanted concentrated The residue is dissolved in 100 ml ether washed with saturated sodium bicarbonate and brine The organic phase is separated dried (MgSO4) concentrated