m-Chloroperbenzoic acid → Diethyl(benzylsulfinylmethyl)phosphonate

HRID 26164노트

반응식

HRID 26164 반응식
[CH2:1]([S:8][CH2:9][P:10](=[O:17])([O:14][CH2:15][CH3:16])[O:11][CH2:12][CH3:13])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.ClC1C=C(C=CC=1)C(OO)=[O:23]>C(Cl)Cl>[CH2:12]([O:11][P:10]([CH2:9][S:8]([CH2:1][C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1)=[O:23])(=[O:17])[O:14][CH2:15][CH3:16])[CH3:13]

참가 물질

4

반응물 2

HCID 70297m-Chloroperbenzoic acidHCID 12536437Diethyl(benzylthiomethyl)phosphonate

생성물 1

HCID 23420192Diethyl(benzylsulfinylmethyl)phosphonate

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

A solution of diethyl (benzylthiomethyl)phosphonate (10 g., 0.036 mole) in 75 ml. of methylene chloride was, with ice-bath cooling, treated with 7.29 g. (0.036 mole) of m-chloroperoxybenzoic acid portionwise. After the addition was complete, the mixture was stirred for 1 hour at ambient temperature, filtered to remove precipitate, and the filtrate concentrated in vacuo. The residue was chromatographed on silica gel by eluting the column with ethyl acetate which gave 5.9 g. of the title compound.

후처리

  1. temperaturecooling
  2. additiontreated with 7.29 g
  3. additionAfter the addition
  4. filtrationfiltered
  5. customto remove precipitate
  6. concentrationthe filtrate concentrated in vacuo
  7. customThe residue was chromatographed on silica gel
  8. washby eluting the column with ethyl acetate which
  9. customgave 5.9 g

출처 및 근거

ORD 기록
ord-59e12b4969a34d26b9ea6fc003a21c40
출처 데이터셋
uspto-grants-1979_04
특허 번호
US04148804

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