N-(3-formylphenyl)methanesulfonamide → [3-(Hydroxyethyl)phenyl](methylsulfonyl)amine
反応式
[CH:1]([C:3]1[CH:4]=[C:5]([NH:9][S:10]([CH3:13])(=[O:12])=[O:11])[CH:6]=[CH:7][CH:8]=1)=[O:2].[CH3:14][Mg]Br>O1CCCC1>[OH:2][CH:1]([C:3]1[CH:4]=[C:5]([NH:9][S:10]([CH3:13])(=[O:12])=[O:11])[CH:6]=[CH:7][CH:8]=1)[CH3:14]参加物
4
実験手順
Under argon and at 0° C., 83 mg (0.417 mmol) of N-(3-formylphenyl)methanesulfonamide (Example 86A) were initially charged in 1 ml of abs. tetrahydrofuran. At 0° C., 99 mg (0.833 mmol) of methylmagnesium bromide (3 M in diethyl ether) were added dropwise (resulting in the formulation of a precipitate), and the reaction solution was stirred at this temperature for 2 h. The reaction solution was quenched with water and extracted three times with ethyl acetate. The combined organic phases were dried over sodium sulfate, filtered and evaporated.
後処理
- customresulting in the formulation of a precipitate), and the reaction solution
- customThe reaction solution was quenched with water
- extractionextracted three times with ethyl acetate
- dry with materialThe combined organic phases were dried over sodium sulfate
- filtrationfiltered
- customevaporated
出典と根拠
- ORDレコード
- ord-9ebb46efaf6049d5b841395a69ffd1af
- 出典データセット
- uspto-grants-2015_11
- 特許番号
- US09187428B2
反応ノート
読み込み中…