反应详情

温度

100 °C

Add 1-azidomethyl-3,5-bis-trifluoromethyl-benzene (1.21 g, 4.5 mmol) to a solution of 4-tributylstannanylethynyl-morpholine in toluene (5 mL) (1.20 g, 3.0 mmol). See Berger, D., et al., Helv. Chim. Acta (1996) 79(I): 179-91. Flush with N2, seal in reaction vessel, and heat at 100° C. overnight. Concentrate, dissolve residue in CHCl3, dry over MgSO4, concentrate. Purify by flash chromatography on silica gel eluting with 0-30% EtOAc/hexanes to afford the title compound (710 mg, 66%); MS(IS) 669 (M+1); TLC: Rf=0.53 (25% EtOAc/hexanes).

1. customFlush with N2
2. customseal in reaction vessel
3. concentrationConcentrate
4. dissolutiondissolve residue in CHCl3
5. dry with materialdry over MgSO4
6. concentrationconcentrate
7. customPurify by flash chromatography on silica gel eluting with 0-30% EtOAc/hexanes