反応 #657275

反応方程式

[2-(2,6-Dimethyl-piperidin-1-yl)acetylamino]-acetic acid

N-Hydroxysuccinimide

N,N′-Dicyclohexyl-carbodiimide

→

[2-(2,6-Dimethyl-piperidin-1-yl)acetylamino]-acetic acid-(2,5-dioxo-pyrrolidine-1-yl)-ester

溶媒

dichloromethane

反応条件

後処理

1. 1
   ろ過The solution was filtered
2. 2
   その他the filtrate was evaporated in vacuo to dryness
3. 3
   workup.DISSOLUTIONThe residue was dissolved in 50 mL dichloromethane
4. 4
   workup.ADDITIONtreated with charcoal
5. 5
   ろ過After filtration
6. 6
   その他the solution was evaporated in vacuo to dryness
7. 7
   その他the product was recrystallised from ethyl acetate

実験手順

4.54 g (20 mMol) [2-(2,6-Dimethyl-piperidin-1-yl)acetylamino]-acetic acid (30) were added to 2.30 g (20 mMol) N-Hydroxysuccinimide and 4.12 g (20 mMol) N,N′-Dicyclohexyl-carbodiimide dissolved in 150 ml dichloromethane. The reaction mixture was stirred for 16 h at room temperature. The solution was filtered and the filtrate was evaporated in vacuo to dryness. The residue was dissolved in 50 mL dichloromethane and treated with charcoal. After filtration, the solution was evaporated in vacuo to dryness and the product was recrystallised from ethyl acetate.

出典