反应 #42134

反应方程式

4-carboxybenzaldehyde

HATU

biphenyl-2-ylcarbamic acid 1-(2-aminoethyl)piperidin-4-yl ester

DIPEA

→

title intermediate

收率 92.2%

Biphenyl-2-ylcarbamic Acid 1-[2-(4-Formylbenzoylamino)ethyl]piperidin-4-yl Ester

收率 92.2%

溶剂

DCM

DCM

反应条件

后处理

1. 1
   workup.STIRRINGThe resulting mixture was stirred at room temperature for 2 hours
2. 2
   洗涤washed with saturated sodium bicarbonate (150 mL) and brine (150 mL)
3. 3
   干燥The organic layer was dried over MgSO4
4. 4
   过滤filtered
5. 5
   浓缩concentrated

实验过程

A mixture of 4-carboxybenzaldehyde (0.95 g, 6.35 mmol) and HATU (3.02 g, 7.94 mmol) in 55 mL of DCM was stirred at room temperature for 1 hour and then biphenyl-2-ylcarbamic acid 1-(2-aminoethyl)piperidin-4-yl ester (3 g, 5.29 mmol; prepared as described in Preparation 7) and DIPEA (4.6 mL, 26.45 mmol) were added. The resulting mixture was stirred at room temperature for 2 hours and then diluted with 100 mL of DCM and washed with saturated sodium bicarbonate (150 mL) and brine (150 mL). The organic layer was dried over MgSO4, filtered and concentrated to provide 2.3 g of the title intermediate (92% yield), which was suitable for use without further purification.

来源