反应 #60017

反应方程式

PyBop

4-acetylbenzoic acid

4-methylmorpholine

TFA

3-methoxybenzylamine

→

(4-acetylphenyl)-N-[(3-methoxyphenyl)methyl]carboxamide

收率 97.0%

溶剂

NMP

dichloromethane

NMP

反应条件

后处理

1. 1
   其他The Sasrin resin was prepared
2. 2
   洗涤The resin was then washed with DMF and dichloromethane

实验过程

The Sasrin resin was prepared as described in Step 2 of Example 3. The resin (500 mg) was heated with a solution of 3-methoxybenzylamine (600 μl ) in NMP (6 ml) at 70° C. for 4 hours. The resin was then washed with DMF and dichloromethane and then shaken with a solution of PyBop® (1.04 g, 2 mmol), 4-acetylbenzoic acid (0.33 g, 2 mmol), 4-methylmorpholine (4 mmol) in NMP (6 ml) at room temperature overnight. A small aliquot of the resin was treated with 20% TFA in dichloromethane to give the intermediate, (4-acetylphenyl)-N-[(3-methoxyphenyl)methyl]carboxamide (HPLC: 23.94 min (97%); MS; MH+=284 (as required)). The resin was then heated at 95° C. for 7 hours in DMFDMA (5 ml).

来源