Hydrochloric Acid → HCID 53729260、化合物

HRID 1591107

反応式

HRID 1591107 の反応式
[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

参加物

5

反応物 3

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

生成物 1

HCID 53729260HCID 53729260、化合物収率 92.5%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-6b216c724d434ab489097d68159381ce
出典データセット
uspto-grants-1993_04
特許番号
US05206259

関連ノート

読み込み中…