Hydrochloric Acid → HCID 53729260, 화합물

HRID 1591107

반응식

HRID 1591107 반응식
[H-].[Al+3].[Li+].[H-].[H-].[H-].[CH3:7][C:8]1[CH:25]=[CH:24][C:11]([S:12][C:13]2[CH:23]=[CH:22][C:16]([C:17](OCC)=[O:18])=[CH:15][CH:14]=2)=[CH:10][CH:9]=1.Cl>O1CCCC1>[CH3:7][C:8]1[CH:25]=[CH:24][C:11]([S:12][C:13]2[CH:23]=[CH:22][C:16]([CH2:17][OH:18])=[CH:15][CH:14]=2)=[CH:10][CH:9]=1

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 10778595Ethyl 4-(4-methylthiophenoxy)benzoateHCID 21226445Aluminium lithium hydride

생성물 1

HCID 53729260HCID 53729260, 화합물수율 92.5%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

To a stirred mixture of lithium aluminum hydride (0.55 g, 14.6 mM) and dry tetrahydrofurane (100 ml) was added a solution (30 ml) of ethyl 4-(4-methylthiophenoxy)benzoate (4.00 g, 14.6 mM) in dry tetrahydrofurane at 0°-10° C., and the mixture was stirred for 12 h at room temperature. To this wa added 10% HCl (200 ml) and the mixture was extracted with toluene. The extract was washed with saturated sodium hydrogen carbonate solution and brine, dried with magnesium sulfate, and concentrated in vacuo. The residue was chromatographed over silica gel to give 4-(4-methylthiophenoxy)benzyl alcohol (3.13 g, 87%) as colorless crystals, m.p. 103.3° C.

후처리

  1. extractionthe mixture was extracted with toluene
  2. washThe extract was washed with saturated sodium hydrogen carbonate solution and brine
  3. dry with materialdried with magnesium sulfate
  4. concentrationconcentrated in vacuo
  5. customThe residue was chromatographed over silica gel

출처 및 근거

ORD 기록
ord-6b216c724d434ab489097d68159381ce
출처 데이터셋
uspto-grants-1993_04
특허 번호
US05206259

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