海萝胶 → 1-(3-Chloro-5-fluoro-4-methoxyphenyl)-1-hexanone

HRID 7894

反应方程式

HRID 7894 反应方程式
[Cl-].[Al+3].[Cl-].[Cl-].[Cl:5][C:6]1[CH:11]=[CH:10][CH:9]=[C:8]([F:12])[C:7]=1[O:13][CH3:14].[C:15](Cl)(=[O:21])[CH2:16][CH2:17][CH2:18][CH2:19][CH3:20].Cl>>[Cl:5][C:6]1[CH:11]=[C:10]([C:15](=[O:21])[CH2:16][CH2:17][CH2:18][CH2:19][CH3:20])[CH:9]=[C:8]([F:12])[C:7]=1[O:13][CH3:14]

参与物

5

实验过程

Aluminum chloride (1.16 g, 8.72 mmol) was added to a stirred mixture of 1-chloro-3-fluoro-2-methoxybenzene (1.00 mL, 8.72 mmol) and hexanoyl chloride (1.47 mL, 10.46 mmol) at room temperature. The mixture warmed and HCl evolution occurred. The resulting mixture was stirred at room temperature for 67 hours and then partitioned between EtOAc (40 mL) and ice cold water (40 mL). The EtOAc layer was washed with brine (30 mL), dried over MgSO4, filtered, and evaporated under vacuum to yield crude 1-(3-chloro-5-fluoro-4-methoxyphenyl)-1-hexanone as an oil.

后处理

  1. temperatureThe mixture warmed
  2. custompartitioned between EtOAc (40 mL) and ice cold water (40 mL)
  3. washThe EtOAc layer was washed with brine (30 mL)
  4. dry with materialdried over MgSO4
  5. filtrationfiltered
  6. customevaporated under vacuum

来源与证据

ORD记录
ord-ec39dbd4e6074985880755ae6356933c
来源数据集
uspto-grants-2006_08
专利号
US07087599B2

关联笔记

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