Dimethylformamide → 1-[(Ethylsulfanyl)methyl]-2-nitrobenzene
反応式
[N+:1]([C:4]1[CH:11]=[CH:10][CH:9]=[CH:8][C:5]=1[CH2:6]Br)([O-:3])=[O:2].CN(C=O)C.[CH2:17]([S-:19])[CH3:18].[Na+]>O>[CH2:17]([S:19][CH2:6][C:5]1[CH:8]=[CH:9][CH:10]=[CH:11][C:4]=1[N+:1]([O-:3])=[O:2])[CH3:18]参加物
5
実験手順
10.0 g (46.3 mmol) of 2-nitrobenzyl bromide were introduced into 100 ml of DMF at 0° C., 3.89 g (46.3 mmol) of sodium ethanethiolate were added in portions, and the mixture was stirred at RT for 4 h. It was diluted with water and extracted with ethyl acetate, and the organic phase was dried over magnesium sulfate, filtered and concentrated. The residue was purified by flash chromatography (mobile phase: cyclohexane/ethyl acetate 9/1) to result in 7.40 g (81% of theory) of the title compound.
後処理
- extractionextracted with ethyl acetate
- dry with materialthe organic phase was dried over magnesium sulfate
- filtrationfiltered
- concentrationconcentrated
- customThe residue was purified by flash chromatography (mobile phase: cyclohexane/ethyl acetate 9/1)
出典と根拠
- ORDレコード
- ord-a2a59b2d0dd64073a9cfbfc157502687
- 出典データセット
- uspto-grants-2011_11
- 特許番号
- US08063234B2
反応ノート
読み込み中…