반응 #929486

반응 방정식

cyclam

Na2CO3

iodopropyltriethoxysilane

→

compound 1

1-[3-(triethoxysilyl)propyl]-1,4,8,11-tetraazacyclotetradecane

용매

acetonitrile

acetonitrile

반응 조건

후처리

1. 1
   온도to reflux
2. 2
   온도the reaction mixture is maintained
3. 3
   온도at reflux for 48 h
4. 4
   기타After evaporating the solvent
5. 5
   기타on a rotary evaporator (still under a nitrogen atmosphere), pentane
6. 6
   workup.ADDITIONis added to the residue
7. 7
   여과the excess cyclam is filtered off
8. 8
   기타the pentane is evaporated

실험 절차

72 g (0.359 mol) of cyclam and 15 g of Na2CO3 (dried at 100° C. under 1 mm Hg for 24 h) are placed in 2.5 l of acetonitrile in a 6 l reactor under a stream of nitrogen. The mixture is brought to reflux, a solution of 24.2 g (0.073 mol) of iodopropyltriethoxysilane in 500 ml of acetonitrile is then added dropwise and then the reaction mixture is maintained at reflux for 48 h. After evaporating the solvent on a rotary evaporator (still under a nitrogen atmosphere), pentane is added to the residue and the excess cyclam is filtered off. This operation is repeated three times, the filtrates are combined, the pentane is evaporated and compound 1 is obtained in the form of a colorless oil (15 g, 50.8%).

출처