反応 #1531300

反応方程式

2,5-dibromo-3-methyl-pyridine

piperazine-1-carboxylic acid tert-butyl ester

DIEA

→

title compound

4-(5-bromo-3-methyl-pyridin-2-yl)-piperazine-1-carboxylic acid tert-butyl ester

溶媒

DMA

反応条件

後処理

1. 1
   その他Partition the dark brown reaction mixture between water and EtOAc
2. 2
   洗浄Wash the EtOAc layer with water (1×) and brine (1×)
3. 3
   乾燥dry (Na2SO4)
4. 4
   濃縮concentrate under reduced pressure
5. 5
   その他to give the crude product
6. 6
   その他Purify by flash chromatography
7. 7
   洗浄eluting with 9:1 hexanes
8. 8
   温度EtOAc, increasing to 3:1 hexanes

実験手順

Heat a solution of 2,5-dibromo-3-methyl-pyridine (Chontech Inc.) (12.6 g, 50.3 mmol), piperazine-1-carboxylic acid tert-butyl ester (11.7 g, 62.9 mmol) and DIEA (13.3 g, 102.0 mmol) in DMA at 130° C. for 36 h. Partition the dark brown reaction mixture between water and EtOAc. Wash the EtOAc layer with water (1×) and brine (1×), dry (Na2SO4) and concentrate under reduced pressure to give the crude product. Purify by flash chromatography, eluting with 9:1 hexanes:EtOAc, increasing to 3:1 hexanes:EtOAc to provide the title compound as a solid.

出典