四氧化硫 → Diethyl 2-carboxybenzylphosphonate

HRID 4916

反应方程式

HRID 4916 反应方程式
C[C:2]1[CH:16]=[CH:15][CH:14]=[CH:13][C:3]=1[CH2:4][P:5](=[O:12])([O:9][CH2:10][CH3:11])[O:6][CH2:7][CH3:8].[O-][Mn](=O)(=O)=O.[K+].[C:23]([O-:26])([O-])=[O:24].[Na+].[Na+].OS(O)(=O)=O>O>[C:23]([C:2]1[CH:16]=[CH:15][CH:14]=[CH:13][C:3]=1[CH2:4][P:5](=[O:12])([O:9][CH2:10][CH3:11])[O:6][CH2:7][CH3:8])([OH:26])=[O:24]

参与物

6

反应物 4

HCID 1118四氧化硫HCID 10340Carbonic acid sodium salt (1:2)HCID 112945(2-甲基苄基)膦酸二乙酯HCID 516875高锰酸钾

产物 1

HCID 11369294Diethyl 2-carboxybenzylphosphonate

试剂、催化剂与溶剂 1

HCID 962聚[6-[4-(4-氰基苯基)苯氧基]己基甲基丙烯酸酯]溶剂

实验过程

4 g of diethyl 2-methylbenzylphosphonate were added to a solution of 12 g of KMnO4 and 4 g of Na2CO3 in 300 ml of water and the mixture was boiled under reflux for 24 hours. It was acidified with 15 ml of concentrated H2SO4 and extracted five times with 300 ml of ether each time. The organic phase was dried over MgSO4, the solvent was evaporated off on a rotary evaporator and the residue was chromatographed over silica gel (CH2Cl2 /methanol/triethylamine 9/1/0.1).

后处理

  1. temperatureunder reflux for 24 hours
  2. extractionextracted five times with 300 ml of ether each time
  3. dry with materialThe organic phase was dried over MgSO4
  4. customthe solvent was evaporated off on a rotary evaporator
  5. customthe residue was chromatographed over silica gel (CH2Cl2 /methanol/triethylamine 9/1/0.1)

来源与证据

ORD记录
ord-3b1908a01a5143ef967011e4244289b7
来源数据集
uspto-grants-1993_09
专利号
US05242908

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