反応 #489936

反応方程式

cesium carbonate

tert-butyl 2-oxo-1-oxa-3,8-diazaspiro[4.5]decane-8-carboxylate

N,N′-dimethylethane-1,2-diamine

methyl 4-bromobenzoate

→

title intermediate

tert-butyl 3-[4-(methoxycarbonyl)phenyl]-2-oxo-1-oxa-3,8-diazaspiro[4.5]decane-8-carboxylate

反応条件

後処理

1. 1
   温度was heated under nitrogen for 18 hours
2. 2
   ろ過The crude mixture was filtered through celite
3. 3
   その他Upon removal of the volatiles
4. 4
   その他the crude was purified by flash chromatography (EtOAc/hexanes 20 to 100%)

実験手順

A mixture of cesium carbonate (4.27 g, 13.11 mmol), copper (I) iodide (0.832 g, 4.37 mmol), tert-butyl 2-oxo-1-oxa-3,8-diazaspiro[4.5]decane-8-carboxylate (1.12 g, 4.37 mmol), N,N′-dimethylethane-1,2-diamine (0.385 g, 437 mmol) and methyl 4-bromobenzoate (1.128 g, 5.24 mmol) was heated under nitrogen for 18 hours. The crude mixture was filtered through celite. Upon removal of the volatiles, the crude was purified by flash chromatography (EtOAc/hexanes 20 to 100%) to afford the title intermediate as a white solid.

出典