4-ethoxybenzenesulfonic Acid → 2-Oxooctyl-p-ethoxybenzene sulfonate

HRID 648231노트

반응식

HRID 648231 반응식
[N+](=[CH:3][C:4](=[O:11])[CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH3:10])=[N-].[CH2:12]([O:14][C:15]1[CH:20]=[CH:19][C:18]([S:21]([OH:24])(=[O:23])=[O:22])=[CH:17][CH:16]=1)[CH3:13]>>[O:11]=[C:4]([CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH3:10])[CH2:3][O:24][S:21]([C:18]1[CH:17]=[CH:16][C:15]([O:14][CH2:12][CH3:13])=[CH:20][CH:19]=1)(=[O:22])=[O:23]

참가 물질

3

반응물 2

HCID 70130204-ethoxybenzenesulfonic AcidHCID 537252081-Diazo-2-octanone

생성물 1

HCID 130032262-Oxooctyl-p-ethoxybenzene sulfonate수율 59%

실험 절차

A 1.0 g quantity of 1-diazo-2-octanone is dissolved in 30 ml of dixoane, and 2.0 g of p-ethoxybenzenesulfonic acid is slowly added to the solution at room temperature. The mixture is stirred until no nitrogen is evolved. The reaction mixture is distilled in a vacuum to remove the solvent, and the residue is extracted with 50 ml of ether, washed with water and dried over anhydrous sodium sulfate. The dried product is distilled in a vacuum to remove the solvent and obtain an oily product, which is purified by column chromatography (silica gel, developer solvent chloroform), affording 1.26 g of 2-oxooctyl-p-ethoxybenzene sulfonate (Compound 46), m.p. 38° to 39° C. Yield 59.0%.

후처리

  1. additionis slowly added to the solution at room temperature
  2. distillationThe reaction mixture is distilled in a vacuum
  3. customto remove the solvent
  4. extractionthe residue is extracted with 50 ml of ether
  5. washwashed with water
  6. dry with materialdried over anhydrous sodium sulfate
  7. distillationThe dried product is distilled in a vacuum
  8. customto remove the solvent
  9. customobtain an oily product, which
  10. customis purified by column chromatography (silica gel, developer solvent chloroform)

출처 및 근거

ORD 기록
ord-ad36fde1397a475fa514be8426a5d9a1
출처 데이터셋
uspto-grants-1983_10
특허 번호
US04411911

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