반응 #567729

반응 방정식

t-butyl bromoacetate

1,4,7,10-tetraazacyclododecane

→

desired compound

수율 99.2%

1,4,7,10-Tetraazacyclododecane-1-acetic acid (1,1dimethylethyl)ester

수율 99.2%

용매

CHCl3

CHCl3

반응 조건

후처리

1. 1
   농축After 14 h the solution was concentrated to 800 mL
2. 2
   세척washed with H2O
3. 3
   기타dried
4. 4
   기타evaporated

실험 절차

A solution of t-butyl bromoacetate (25.3 g; 130 mmol) in CHCl3 (500 mL) (commercial product) was added dropwise in 7 h to a solution of 1,4,7,10-tetraazacyclododecane (112.3 g; 650 mmol) (commercial product) in CHCl3 (2 L) maintained under nitrogen at room temperature. After 14 h the solution was concentrated to 800 mL, washed with H2O, dried and evaporated to give the desired compound (39 g; 129 mmol). Yield 99%. GC: 92% (area %). K.F.: 0.42%. The 13C-NMR, MS and IR spectra were consistent with the structure.

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