反应详情

Add slowly a solution of 2-naphthoyl chloride (600 mg, 3.15 mmol) to a solution of 4-[4-(6-fluoro-benzo[b]thiophen-3-yl)-[1,4]diazapan-1-yl]butylamine (Example 6) (920 mg, 2.86 mmol), in pyridine-methylene chloride (10 mL,1:1), and stir the solution at room temperature overnight. Evaporate the solvent under vacuum, dissolve the residue in EtOAc and wash the organic layer with water and saturated sodium chloride solution. Combine the organic phases, dry over MgSO4 and evaporate the solvent under vacuum. Purify the crude product by column chromatography (EtOAc/MeOH 7:3) to obtain 1.25 g of a solid LC/MS (LiChrospher 5μ, RP-18, 250 mm CH3CN/Water-gradient 20%→100% (25 min), Flow: 1.5 mL/min) tR=21.11 min, m/z=475.3.

1. customEvaporate the solvent under vacuum
2. dissolutiondissolve the residue in EtOAc
3. washwash the organic layer with water and saturated sodium chloride solution
4. dry with materialCombine the organic phases, dry over MgSO4
5. customevaporate the solvent under vacuum
6. customPurify the crude product by column chromatography (EtOAc/MeOH 7:3)