甲基硫酸酯-13C2 → 4-甲氧基水杨酸甲酯

HRID 256337

反应方程式

HRID 256337 反应方程式
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([OH:12])[C:6](=[CH:10][CH:11]=1)[C:7]([OH:9])=[O:8].[C:13](=O)(O)[O-].[Na+].S(OC)(OC)(=O)=O>CC(C)=O.CCOCC.C1(C)C=CC=CC=1>[CH3:13][O:8][C:7](=[O:9])[C:6]1[C:5](=[CH:4][C:3]([O:2][CH3:1])=[CH:11][CH:10]=1)[OH:12]

参与物

7

反应物 3

HCID 6497甲基硫酸酯-13C2HCID 752314-甲氧基水杨酸HCID 516892碳酸氢钠

产物 1

HCID 795234-甲氧基水杨酸甲酯收率 98,858.797%

试剂、催化剂与溶剂 3

HCID 180丙酮溶剂HCID 1140甲苯溶剂HCID 3283乙醚溶剂

实验过程

A mixture of 4-methoxysalicylic acid (Aldrich) (178.1 g, 1.06 mmole) sodium bicarbonate (89 g, 1.06 mole), and dimethyl sulfate (133.6 g, 1.06 mole) in acetone (2 l) is refluxed with stirring under nitrogen for 20 hours. The mixture is cooled, filtered, and the acetone is removed under reduced pressure to yield an oily residue. The residue is taken up in ether (1.8 l) and toluene (0.50 l). The extracts are washed with sodium bicarbonate solution, water, dried over sodium sulfate, and concentrated to give a syrup (190.9 g). Recrystallization from hexane gives 172.7 g (89.5%) of analytically pure solid, mp 49°-50° C.

后处理

  1. temperatureis refluxed
  2. temperatureThe mixture is cooled
  3. filtrationfiltered
  4. customthe acetone is removed under reduced pressure
  5. customto yield an oily residue
  6. washThe extracts are washed with sodium bicarbonate solution, water
  7. dry with materialdried over sodium sulfate
  8. concentrationconcentrated

来源与证据

ORD记录
ord-f7f85d8a445d4379b1ab9d2dff21c91b
来源数据集
uspto-grants-1987_10
专利号
US04703053

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