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

HRID 1450310

반응식

HRID 1450310 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 241Benzene용매

실험 절차

To a mixture 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.

후처리

  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

출처 및 근거

ORD 기록
ord-410c7e0886004c46b86f1c1c68aec268
출처 데이터셋
uspto-grants-1997_02
특허 번호
US05602118

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