Реакция #567729

Уравнение реакции

t-butyl bromoacetate

1,4,7,10-tetraazacyclododecane

→

desired compound

Выход 99.2%

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

Выход 99.2%

Растворители

CHCl3

CHCl3

Условия реакции

Обработка

1. 1
   КонцентрированиеAfter 14 h the solution was concentrated to 800 mL
2. 2
   Промывкаwashed with H2O
3. 3
   Другоеdried
4. 4
   Другоеevaporated

Методика

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.

Источник