Methanesulfonyl chloride → HCID 86672755、化合物
反応式
[Br:1][C:2]1[CH:7]=[C:6]([CH2:8][OH:9])[CH:5]=[CH:4][N:3]=1.CCN(C(C)C)C(C)C.[CH3:19][S:20](Cl)(=[O:22])=[O:21]>ClCCl>[Br:1][C:2]1[CH:7]=[C:6]([CH2:8][O:9][S:20]([CH3:19])(=[O:22])=[O:21])[CH:5]=[CH:4][N:3]=1参加物
5
実験手順
To a chilled (0° C.) solution of (2-bromopyridin-4-yl)-methanol (3.00 g, 16.0 mmol) and DIPEA (8.3 mL, 48 mmol) in dichloromethane (30 mL) is added methanesulfonyl chloride (1.30 mL, 16.8 mmol). The resulting mixture is warmed to room temperature. After 1 hour, the mixture is diluted with dichloromethane (20 mL) and washed with saturated aqueous ammonium chloride (3×10 mL), saturated aqueous sodium bicarbonate (10 mL) and brine (10 mL), dried over MgSO4, filtered and concentrated to afford crude methanesulfonic acid 2-bromopyridin-4-ylmethyl ester, which is used without purification.
後処理
- washwashed with saturated aqueous ammonium chloride (3×10 mL), saturated aqueous sodium bicarbonate (10 mL) and brine (10 mL)
- dry with materialdried over MgSO4
- filtrationfiltered
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-a69dc61edfa6485bbaf7074045cc9895
- 出典データセット
- uspto-grants-2015_01
- 特許番号
- US08927550B2
反応ノート
読み込み中…