反应 #66552

反应方程式

TFA

ethyl JV-benzylglycinate

DCC

aminobutyric acid

→

title compound

(3S)-3-Ethyl-1-(phenylmethyl)-2,5-piperazinedione

溶剂

DCM

DCM

反应条件

后处理

1. 1
   过滤filtered
2. 2
   浓缩the concentrated
3. 3
   其他to give an oil
4. 4
   浓缩The solution was concentrated under reduced pressure
5. 5
   workup.STIRRINGThe residue was stirred in saturated aq NaHCO3 (125 ml)
6. 6
   workup.WAITEtOAc (125 ml) for 6 h
7. 7
   其他The organics were separated
8. 8
   干燥dried (Na2SO4)
9. 9
   浓缩concentrated

实验过程

To a solution of DCC (5.07 g) in DCM (140 mL) at 0° C. was added N—BOC-L-□-aminobutyric acid (5 g) followed by ethyl JV-benzylglycinate (4.6 mL) dropwise. The resulting solution was stirred at 0° C. for 2 h and RT 1 h, filtered and the concentrated to give an oil. This was dissolved in DCM (100 mL) and TFA (100 ml) and stirred for 1 h. The solution was concentrated under reduced pressure. The residue was stirred in saturated aq NaHCO3 (125 ml) and EtOAc (125 ml) for 6 h. The organics were separated, dried (Na2SO4), and concentrated to give the sub title compound as a white solid. (5.68 g).

来源