Sulfuric Acid → Diethyl 2-carboxybenzylphosphonate

HRID 4916

反応式

HRID 4916 の反応式
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]

参加物

6

反応物 4

HCID 1118Sulfuric AcidHCID 10340Sodium CarbonateHCID 112945Phosphonic acid, P-((2-methylphenyl)methyl)-, diethyl esterHCID 516875Potassium Permanganate

生成物 1

HCID 11369294Diethyl 2-carboxybenzylphosphonate

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

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).

後処理

  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)

出典と根拠

ORDレコード
ord-3b1908a01a5143ef967011e4244289b7
出典データセット
uspto-grants-1993_09
特許番号
US05242908

関連ノート

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