反应 #2886295
相关文献 (1)
openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US06652834B2
反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: 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. After 14 h the solution was concentrated to 800 mL washed with H2O dried evaporated
来源 ID: ord-14049639a5fd4a40a7a050ed3cb12457