氯甲基甲基醚 → Ethyl 3-bromo-4-methoxymethoxybenzoate

HRID 13259

反应方程式

HRID 13259 反应方程式
[H-].[Na+].[O:3]1[CH2:7]CC[CH2:4]1.[Br:8][C:9]1[CH:10]=[C:11]([CH:17]=[CH:18][C:19]=1[OH:20])[C:12]([O:14][CH2:15][CH3:16])=[O:13].COCCl>C(OCC)(=O)C>[Br:8][C:9]1[CH:10]=[C:11]([CH:17]=[CH:18][C:19]=1[O:20][CH2:4][O:3][CH3:7])[C:12]([O:14][CH2:15][CH3:16])=[O:13]

参与物

6

反应物 4

HCID 7864氯甲基甲基醚HCID 8028四氢呋喃HCID 24758氢化钠HCID 47789643-溴-4-羟基苯甲酸乙酯

产物 1

HCID 23145548Ethyl 3-bromo-4-methoxymethoxybenzoate

试剂、催化剂与溶剂 1

HCID 8857乙酸乙酯溶剂

实验过程

5.5 g of sodium hydride was added to a tetrahydrofuran (300 ml) solution of 20.5 g of ethyl 3-bromo-4-hydroxybenzoate produced according to the method described in Monatsh. Chem.; 22; 1901; 437, with cooling with ice, and the reaction liquid was stirred for 30 minutes, and then, at the same temperature, 10 ml of chloromethyl methyl ether was added to the reaction liquid, and the reaction liquid was stirred overnight at room temperature. The reaction liquid was diluted with ethyl acetate, and washed with water, and the aqueous layer was extracted with ethyl acetate, and dried with anhydrous magnesium sulfate. The solvent was evaporated away under reduced pressure, and the resulting solid was suspended in hexane and then taken out through filtration to obtain the entitled compound as a white solid.

后处理

  1. customproduced
  2. temperature437, with cooling with ice
  3. customthe reaction liquid
  4. customthe reaction liquid
  5. stirringwas stirred overnight at room temperature
  6. customThe reaction liquid
  7. washwashed with water
  8. extractionthe aqueous layer was extracted with ethyl acetate
  9. dry with materialdried with anhydrous magnesium sulfate
  10. customThe solvent was evaporated away under reduced pressure
  11. filtrationtaken out through filtration

来源与证据

ORD记录
ord-39773446c1b64b71b3c66c90f66f485a
来源数据集
uspto-grants-2010_06
专利号
US07728025B2

关联笔记

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