反応 #657271

反応方程式

(2,6-Dimethyl-piperidin-1-yl)-acetic acid hydrochloride

(2,6-Dimethyl-piperidine-1-yl)-acetic acid hydrochloride

N-hydroxysuccinimide

→

(2,6-Dimethyl-piperidine-1-yl)-acetic acid-(2,5-dioxo-pyrrolidine-1-yl)-ester

溶媒

DMF

反応条件

後処理

1. 1
   ろ過The residue was filtered
2. 2
   その他the filtrate was evaporated in vacuo to dryness
3. 3
   workup.DISSOLUTIONAfter dissolving the residue in 300 ml CH2Cl2
4. 4
   洗浄the solution was washed with NaHCO3
5. 5
   乾燥dried over sodium sulphate
6. 6
   その他the solvent was evaporated
7. 7
   その他The compound was then recrystallised from diisopropylether (activated charcoal)

実験手順

12.60 g (60 mMol) (2,6-Dimethyl-piperidin-1-yl)-acetic acid hydrochloride (5), in 100 ml DMF, was added to 7.02 g (60 mMol) N-hydroxysuccinimide and 12.58 g (60 mMol) N,N-dicyclohexylcarbodiimide. The reaction mixture was stirred for 16 h at RT. The residue was filtered and the filtrate was evaporated in vacuo to dryness. After dissolving the residue in 300 ml CH2Cl2, the solution was washed with NaHCO3, dried over sodium sulphate and the solvent was evaporated. The compound was then recrystallised from diisopropylether (activated charcoal).

出典