Pyrrolidine → HCID 75480723、化合物
反応式
Br[C:2]1[CH:3]=[CH:4][C:5]([N+:8]([O-:10])=[O:9])=[N:6][CH:7]=1.[NH:11]1[CH2:15][CH2:14][CH2:13][CH2:12]1>O>[N+:8]([C:5]1[CH:4]=[CH:3][C:2]([N:11]2[CH2:15][CH2:14][CH2:13][CH2:12]2)=[CH:7][N:6]=1)([O-:10])=[O:9]参加物
4
反応条件
- 温度
- 120 °C
実験手順
A mixture of 600 mg (2.93 mmol) of 5-bromo-2-nitropyridine and 1.05 g (14.63 mmol) of pyrrolidine is heated in a Biotage microwave machine for 1 hour at 120° C. The reaction medium is diluted with water and then extracted with ethyl acetate. The organic phase is washed twice with water, dried over MgSO4 and then filtered. The filtrate is evaporated under reduced pressure and then chromatographed on silica gel, eluting with a heptane/ethyl acetate mixture from (100/0 v/v) up to (50/50 v/v) to give 410 mg of 2-nitro-5-pyrrolidin-1-ylpyridine.
後処理
- extractionextracted with ethyl acetate
- washThe organic phase is washed twice with water
- dry with materialdried over MgSO4
- filtrationfiltered
- customThe filtrate is evaporated under reduced pressure
- customchromatographed on silica gel
- washeluting with a heptane/ethyl acetate mixture from (100/0 v/v) up to (50/50 v/v)
出典と根拠
- ORDレコード
- ord-1d08bca20e5545d0b70ccbdc23196acb
- 出典データセット
- uspto-grants-2015_09
- 特許番号
- US09120812B2
反応ノート
読み込み中…