反応 #86215

反応方程式

tert-butyl N-[(3S)-1-[3-chloro-6-[6-(6-methylpyrazin-2-yl)pyrazolo[4,3-c]pyridin-1-yl]pyrazin-2-yl]-3-piperidyl]carbamate

trifluoroacetic acid

→

226

収率 49.9%

(3S)-1-[3-chloro-6-[6-(6-methylpyrazin-2-yl)pyrazolo[4,3-c]pyridin-1-yl]pyrazin-2-yl]piperidin-3-amine

収率 49.9%

溶媒

dichloromethane

反応条件

後処理

1. 1
   濃縮The reaction was concentrated
2. 2
   workup.ADDITIONdiluted with water
3. 3
   抽出then extracted with EtOAc
4. 4
   抽出then extracted with EtOAc
5. 5
   乾燥The organic layers was dried with sodium sulfate
6. 6
   ろ過filtered
7. 7
   濃縮concentrated in vacuum

実験手順

A solution of tert-butyl N-[(3S)-1-[3-chloro-6-[6-(6-methylpyrazin-2-yl)pyrazolo[4,3-c]pyridin-1-yl]pyrazin-2-yl]-3-piperidyl]carbamate (30 mg, 0.057 mmol) in dichloromethane 4.0 ml and trifluoroacetic acid (0.80 ml, 10 mmol) was stirred at RT 3 h. The reaction was concentrated and diluted with water then extracted with EtOAc. The aqueous layer was basified with 1M NaOH to pH 10 then extracted with EtOAc. The organic layers was dried with sodium sulfate, filtered, and concentrated in vacuum. The crude product was submitted for reverse phase HPLC to give 226 (12 mg, 49% yield). MS (ESI) m/z: 422.1.

出典