p-Toluenesulfonic acid → Acetic acid, (dimethoxyphosphinyl)hydroxy-, (4-nitrophenyl)methyl ester

HRID 54782

反応式

HRID 54782 の反応式
[C:1]([O:5][CH2:6][C:7]1[CH:12]=[CH:11][C:10]([N+:13]([O-:15])=[O:14])=[CH:9][CH:8]=1)(=[O:4])[CH:2]=[O:3].[CH3:16][O:17][P:18]([O-:21])[O:19][CH3:20].C1(C)C=CC(S(O)(=O)=O)=CC=1>C1C=CC=CC=1>[N+:13]([C:10]1[CH:11]=[CH:12][C:7]([CH2:6][O:5][C:1](=[O:4])[CH:2]([P:18]([O:19][CH3:20])([O:17][CH3:16])=[O:21])[OH:3])=[CH:8][CH:9]=1)([O-:15])=[O:14]

参加物

5

反応物 3

HCID 6101p-Toluenesulfonic acidHCID 12544839(4-Nitrophenyl)methyl oxoacetateHCID 21884954Dimethylphosphite

生成物 1

HCID 10064522Acetic acid, (dimethoxyphosphinyl)hydroxy-, (4-nitrophenyl)methyl ester

試薬・触媒・溶媒 1

HCID 241Benzene溶媒

実験手順

To a minute of 4.32 g of p-nitrobenzyl glyoxalate and 2.0 ml of dimethylphosphite in 25 ml of benzene is added a catalytic amount of p-toluenesulfonic acid. The reaction is heated at reflux temperature for 1.5 hours. The formed water is removed using a Dean-Stark trap. After cooling, the solvent is removed in vacuo and the resulting crystals are slurried in ethyl acetate and collected to give 3.48 g of the desired product.

後処理

  1. temperatureThe reaction is heated
  2. temperatureat reflux temperature for 1.5 hours
  3. customThe formed water is removed
  4. temperatureAfter cooling
  5. customthe solvent is removed in vacuo
  6. customcollected

出典と根拠

ORDレコード
ord-3593bab6bf7743fba427e05b69193bd6
出典データセット
uspto-grants-1997_04
特許番号
US05623081

関連ノート

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