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Sulfuric Acid → HCID 21258641, 화합물

HRID 617603
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HRID 617603 반응식
S(=O)(=O)(O)[OH:2].[CH2:6]([O:13][CH2:14][CH2:15][C:16]([CH2:28][CH2:29][C:30]1[CH:35]=[CH:34][CH:33]=[CH:32][CH:31]=1)(O)[CH2:17][CH2:18][O:19][CH2:20][C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1)[C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1.[C:36](#[N:38])[CH3:37]>>[CH2:6]([O:13][CH2:14][CH2:15][C:16]([NH:38][C:36](=[O:2])[CH3:37])([CH2:17][CH2:18][O:19][CH2:20][C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1)[CH2:28][CH2:29][C:30]1[CH:35]=[CH:34][CH:33]=[CH:32][CH:31]=1)[C:7]1[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 3

HCID 1118Sulfuric AcidHCID 6342AcetonitrileHCID 22618832HCID 22618832, 화합물

생성물 1

HCID 21258641HCID 21258641, 화합물

실험 절차

Sulfuric acid (4.2 g) was added to a solution of 1,5-dibenzyloxy-3-(2-phenylethyl)-3-pentanol (5.8 g) in acetonitrile (50 ml) under ice-cooling and the mixture was stirred at room temperature for 3 hours. The mixture was poured into ice-water and extracted with ethyl acetate. The ethyl acetate layer was washed with a saturated aqueous sodium hydrogencarbonate solution and a saturated brine, dried over anhydrous sodium sulfate and concentrated. The residue obtained was purified by silica gel column chromatography (eluent; n-hexane:ethyl acetate=7:3) to give the subject compound (2.2 g) as a yellowish oily substance.

후처리

  1. temperature
cooling
  • extractionextracted with ethyl acetate
  • washThe ethyl acetate layer was washed with a saturated aqueous sodium hydrogencarbonate solution
  • dry with materiala saturated brine, dried over anhydrous sodium sulfate
  • concentrationconcentrated
  • customThe residue obtained
  • customwas purified by silica gel column chromatography (eluent; n-hexane:ethyl acetate=7:3)
  • 출처 및 근거

    ORD 기록
    ord-5914c373f4164fa5bba58383a818d056
    출처 데이터셋
    uspto-grants-1999_09
    DOI
    10.6084/m9.figshare.5104873.v1
    특허 번호
    US05948820

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