Propargyl bromide → 1-[(Prop-2-yn-1-yl)oxy]-2-(trifluoromethyl)benzene
反応式
[F:1][C:2]([F:11])([F:10])[C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[OH:9].[CH:12]#[C:13][CH2:14]Br.C([O-])([O-])=O.[K+].[K+]>C(#N)C>[CH2:14]([O:9][C:4]1[CH:5]=[CH:6][CH:7]=[CH:8][C:3]=1[C:2]([F:10])([F:11])[F:1])[C:13]#[CH:12]参加物
5
実験手順
To a stirred solution of 2-(trifluoromethyl)phenol (50.0 g, 0.31 mol) and progargyl bromide (44.0 g, 0.37 mol) in ACN (500 mL) was added K2CO3 (51.0 g, 0.37 mol) and the mixture was stirred overnight at rt, concentrated, diluted with water and extracted with Et2O. The combined organic layers were dried over Na2SO4, filtered, concentrated and purified by CC (PE/EA=40/1) to give compound P33a (59.7 g, 97%) as an oil.
後処理
- concentrationconcentrated
- additiondiluted with water
- extractionextracted with Et2O
- dry with materialThe combined organic layers were dried over Na2SO4
- filtrationfiltered
- concentrationconcentrated
- custompurified by CC (PE/EA=40/1)
- customto give compound P33a (59.7 g, 97%) as an oil
出典と根拠
- ORDレコード
- ord-7153c67ecf21467cbf3c81b45529fe39
- 出典データセット
- uspto-grants-2015_02
- 特許番号
- US08946446B2
反応ノート
読み込み中…