海萝胶 → 2,4-二甲氧基苯甲酸甲酯

HRID 501784

反应方程式

HRID 501784 反应方程式
OC1C=[C:9]([OH:11])[CH:8]=[CH:7][C:3]=1[C:4](O)=O.[C:12](=O)([O-])[O-].[K+].[K+].S([O:23][CH3:24])(OC)(=O)=O.Cl.[C:26]([O:29][CH2:30]C)(=[O:28])[CH3:27]>O.CN(C)C=O>[CH3:12][O:11][C:9]1[CH:8]=[C:7]([O:23][CH3:24])[CH:3]=[CH:4][C:27]=1[C:26]([O:29][CH3:30])=[O:28]

参与物

8

反应物 5

HCID 313海萝胶HCID 14912,4-二羟基苯甲酸HCID 6497甲基硫酸酯-13C22 次HCID 8857乙酸乙酯HCID 11430碳酸钾2 次

产物 1

HCID 1374512,4-二甲氧基苯甲酸甲酯

试剂、催化剂与溶剂 2

HCID 962聚[6-[4-(4-氰基苯基)苯氧基]己基甲基丙烯酸酯]溶剂HCID 6228N,N-二甲基甲酰胺溶剂

反应条件

温度
75 °C

实验过程

50 g of 2,4-dihydroxybenzoic acid, 269 g of potassium carbonate, 123 mL of dimethyl sulfate, and 500 mL of N,N-dimethylformamide were suspended together, and this suspension was stirred for 6.5 hours at 70 to 80° C. Further, 90 g of potassium carbonate and 61 mL of dimethyl sulfate were added to this suspension, which was stirred for another 4 hours at 110 to 115° C. This reaction mixture was added to a mixture of ethyl acetate and water, and adjusted to pH 2 with 6M hydrochloric acid, and then the organic phase was separated therefrom. After the resultant organic phase was washed with water and a saturated sodium chloride solution successively, the washed phase was dried over anhydrous magnesium sulfate, and the solvent was distilled out under reduced pressure. The resultant residue was purified by silica gel column chromatography [eluent; hexane:ethyl acetate=1:2] to yield 54 g of methyl 2,4-dimethoxybenzoate as yellow oil.

后处理

  1. stirringwas stirred for another 4 hours at 110 to 115° C
  2. customthe organic phase was separated
  3. washAfter the resultant organic phase was washed with water
  4. dry with materiala saturated sodium chloride solution successively, the washed phase was dried over anhydrous magnesium sulfate
  5. distillationthe solvent was distilled out under reduced pressure
  6. customThe resultant residue was purified by silica gel column chromatography [eluent; hexane:ethyl acetate=1:2]

来源与证据

ORD记录
ord-fb59e1c798564fa39839988088ff206f
来源数据集
uspto-grants-2010_08
专利号
US07772285B2

关联笔记

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