Cesium carbonate → 3-(3-Bromophenylsulfanyl)propane-1-ol
반응식
[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]=1참가 물질
5
반응 조건
- 온도
- 50 °C
실험 절차
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.
후처리
- distillationDMF was distilled out completely
- dissolutionthe residue was dissolved in DCM
- washwashed with water, brine
- dry with materialdried over Na2SO4
- customThe solvent was evaporated
출처 및 근거
- ORD 기록
- ord-9bf8661431e24bdfbc49231fe41400a2
- 출처 데이터셋
- uspto-grants-2012_09
- 특허 번호
- US08273769B2
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