反应 #554663

反应方程式

6-[(4-fluoro-3-methylphenoxy)methyl]-2-methylazepane

5-methyl-2-(2H-1,2,3-triazol-2-yl)benzoic acid

EDC

HOBT

triethylamine

→

6-[(4-fluoro-3-methylphenoxy)methyl]-2-methyl-1-[5-methyl-2-(2H-1,2,3-triazol-2-yl)benzoyl]azepane

溶剂

DMF

反应条件

后处理

1. 1
   过滤The mixture was filtered
2. 2
   其他purified by reverse phase liquid chromatography (Sunfire C18 OBD 5 um, 20×150 mm column; 0-100% CH3CN/H2O gradient w/0.10% TFA present)

实验过程

A solution of 6-[(4-fluoro-3-methylphenoxy)methyl]-2-methylazepane (2-7, 50 mg, 0.20 mmol, 1.0 equiv) in DMF (3 mL) was treated with 5-methyl-2-(2H-1,2,3-triazol-2-yl)benzoic acid (45 mg, 0.22 mmol, 1.1 equiv), EDC (46 mg, 0.24 mmol, 1.2 equiv), HOBT (37 mg, 0.24 mmol, 1.2 equiv) and triethylamine (83 ul, 60 mg, 0.60 mmol, 3.0 equiv) and the resulting mixture was stirred at 23° C. for 16 hours. The mixture was filtered and purified by reverse phase liquid chromatography (Sunfire C18 OBD 5 um, 20×150 mm column; 0-100% CH3CN/H2O gradient w/0.10% TFA present) to yield 6-[(4-fluoro-3-methylphenoxy)methyl]-2-methyl-1-[5-methyl-2-(2H-1,2,3-triazol-2-yl)benzoyl]azepane (2-8). δ 7.95-6.14 (m, 8H), 4.97-0.65 (m, 21H). LRMS m/z (M+H) 437.4 found, 437.2 required.

来源