Cesium carbonate → 3-(3-Bromophenylsulfanyl)propane-1-ol
反応式
[Br:1][C:2]1[CH:3]=[C:4]([SH:8])[CH:5]=[CH:6][CH:7]=1.C([O-])([O-])=O.[Cs+].[Cs+].Br[CH2:16][CH2:17][CH2:18][OH:19]>CN(C=O)C>[Br:1][C:2]1[CH:3]=[C:4]([S:8][CH2:16][CH2:17][CH2:18][OH:19])[CH:5]=[CH:6][CH:7]=1参加物
5
反応条件
- 温度
- 50 °C
実験手順
A solution of 3-bromobenzenethiol (5.00 g, 26.4 mmol) in anhydrous DMF (30 mL) was treated with Cs2CO3 (17.2 g, 52.9 mmol) followed by 3-bromopropan-1-ol (4.40 g, 31.6 mmol). The mixture was heated to 50° C. under nitrogen for 12 h. DMF was distilled out completely, and the residue was dissolved in DCM and washed with water, brine and dried over Na2SO4. The solvent was evaporated to afford 6.4 g (98%) of the title compound as pale yellow liquid.
後処理
- distillationDMF was distilled out completely
- dissolutionthe residue was dissolved in DCM
- washwashed with water, brine
- dry with materialdried over Na2SO4
- customThe solvent was evaporated
出典と根拠
- ORDレコード
- ord-9bf8661431e24bdfbc49231fe41400a2
- 出典データセット
- uspto-grants-2012_09
- 特許番号
- US08273769B2
反応ノート
読み込み中…