反応 #1898148
ord-8b8d07f68af74df58478088be04b392d
反応方程式
4-(5-chloro-3-nitro-pyridin-2-yl)-piperazine-1-carboxylic acid tert-butyl ester
ethyl acetate
→
4-(3-amino-5-chloro-pyridin-2-yl)-piperazine-1-carboxylic acid tert-butyl ester
収率 80.0%
溶媒
反応条件
詳細条件
See reaction.notes.procedure_details.
後処理
- 1その他The flask was evacuated
- 2workup.ADDITIONrefilled with argon three times
- 3ろ過The mixture is filtered through a pad of diatomaceous earth
- 4濃縮concentrated under reduced pressure
実験手順
A round bottom flask is charged with 5% platinum sulfide on carbon (0.20 g, 0.039 mmol). The flask was evacuated and refilled with argon three times. To the flask is added 4-(5-chloro-3-nitro-pyridin-2-yl)-piperazine-1-carboxylic acid tert-butyl ester (2.80 g, 8.17 mmol) as a solution in a 1:1 mixture of ethyl acetate:methanol (100 mL). The mixture is placed under an atmosphere of hydrogen and stirred overnight at room temperature. The mixture is filtered through a pad of diatomaceous earth and concentrated under reduced pressure to provide 2.0 g of 4-(3-amino-5-chloro-pyridin-2-yl)-piperazine-1-carboxylic acid tert-butyl ester as a dark solid in 80% yield.