肉桂醛 → alpha-溴代肉桂醛

HRID 555974

反应方程式

HRID 555974 反应方程式
[CH:1](=[O:10])[CH:2]=[CH:3][C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1.[Br:11]Br.C([O-])([O-])=O.[K+].[K+].O>C(O)(=O)C>[Br:11][C:2](=[CH:3][C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1)[CH:1]=[O:10]

参与物

6

实验过程

1.33 g (10 mmol) cinnamaldehyde was dissolved in 5 mL glacial acetic acid and cooled on an ice-water bath. 1.62 g bromine was added, and anhydrous K2CO3 was then added, and it was stirred until no gas was evolving. After refluxing for 30 min, the reaction mixture was poured into 100 mL cold water with stirring, extracted with 50 mL ethyl ether three times. The combined ethyl ether layers were washed with water one time, saturated aqueous NaCl solution one time, dried over MgSO4 for 2 hours, filtrated, and the filtrate was dried under vacuum, and washed with anhydrous ethyl ether: petroleum ether (1:1) to give the title compound as light yellow powder.

后处理

  1. temperaturecooled on an ice-water bath
  2. temperatureAfter refluxing for 30 min
  3. stirringwith stirring
  4. extractionextracted with 50 mL ethyl ether three times
  5. washThe combined ethyl ether layers were washed with water one time, saturated aqueous NaCl solution one time
  6. dry with materialdried over MgSO4 for 2 hours
  7. filtrationfiltrated
  8. customthe filtrate was dried under vacuum
  9. washwashed with anhydrous ethyl ether: petroleum ether (1:1)

来源与证据

ORD记录
ord-33127781f18340369da56dfe4b8793c5
来源数据集
uspto-grants-2011_11
专利号
US08053577B2

关联笔记

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