3-羟基苯甲醇 → [3-(2-Methoxyethoxy)phenyl]methanol

HRID 45228

反应方程式

HRID 45228 反应方程式
[OH:1][CH2:2][C:3]1[CH:4]=[C:5]([OH:9])[CH:6]=[CH:7][CH:8]=1.C([O-])([O-])=O.[Cs+].[Cs+].[CH3:16][O:17][CH2:18][CH2:19]Br>CC#N>[CH3:16][O:17][CH2:18][CH2:19][O:9][C:5]1[CH:4]=[C:3]([CH2:2][OH:1])[CH:8]=[CH:7][CH:6]=1

参与物

5

反应物 3

HCID 1023-羟基苯甲醇HCID 10796碳酸氢铯HCID 809722-溴乙基甲基醚

产物 1

HCID 20110194[3-(2-Methoxyethoxy)phenyl]methanol

试剂、催化剂与溶剂 1

HCID 6342乙腈溶剂

反应条件

温度
110 °C

实验过程

A mixture of 10 g (80.6 mmol) of 3-(hydroxymethyl)phenol, 78.4 g (241.7 mmol) of Cs2CO3 and 8.4 mL (88.6 mmol) of bromoethyl methyl ether in 150 mL of CH3CN is heated for 12 hours at 110° C. After cooling to room temperature, the medium is filtered, concentrated under reduced pressure, taken up in 500 mL of DCM, washed with brine (2×100 mL) dried over Na2SO4, filtered and then concentrated under reduced pressure. 10.9 g of 3-(2-methoxyethoxy)phenyl]methanol are obtained in the form of a yellow oil.

后处理

  1. temperatureAfter cooling to room temperature
  2. filtrationthe medium is filtered
  3. concentrationconcentrated under reduced pressure
  4. washwashed with brine (2×100 mL)
  5. dry with materialdried over Na2SO4
  6. filtrationfiltered
  7. concentrationconcentrated under reduced pressure
  8. custom10.9 g of 3-(2-methoxyethoxy)phenyl]methanol are obtained in the form of a yellow oil

来源与证据

ORD记录
ord-508484e1afec43eb83cbb806dec4e237
来源数据集
uspto-grants-2013_09
专利号
US08541455B2

关联笔记

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