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Chloroform → 2-[1-(2-tert-Butyldiphenylsiloxyethyl)cyclohexyl]ethanol

HRID 2223854
ノート
印刷プレビュー

反応式

HRID 2223854 の反応式
[OH:1][CH2:2][CH2:3][C:4]1([CH2:10][CH2:11][OH:12])[CH2:9][CH2:8][CH2:7][CH2:6][CH2:5]1.C(N(CC)CC)C.[C:20]([Si:24]([C:32]1[CH:37]=[CH:36][CH:35]=[CH:34][CH:33]=1)([C:26]1[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=1)Cl)([CH3:23])([CH3:22])[CH3:21].C(Cl)(Cl)Cl>ClCCl>[O:1]([CH2:2][CH2:3][C:4]1([CH2:10][CH2:11][OH:12])[CH2:5][CH2:6][CH2:7][CH2:8][CH2:9]1)[Si:24]([C:20]([CH3:23])([CH3:22])[CH3:21])([C:32]1[CH:33]=[CH:34][CH:35]=[CH:36][CH:37]=1)[C:26]1[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 6212ChloroformHCID 8471TriethylamineHCID 76657Cyclohexane-1,1-diethanolHCID 94078tert-Butyldiphenylchlorosilane

生成物 1

HCID 574278602-[1-(2-tert-Butyldiphenylsiloxyethyl)cyclohexyl]ethanol

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a solution of 2-[1-(2-hydroxyethyl)cyclohexyl]ethanol (6.41 g) in dichloromethane (170 mL) were added triethylamine (6.74 mL) and tert-butyldiphenylchlorosilane (11.1 mL) at room temperature. After stirring the solution at room temperature for 18 hours, chloroform was added to the solution, and it was washed in turn with 1N hydrochloric acid, saturated aqueous sodium bicarbonate solution and saturated aqueous sodium chloride solution. The solution was dried over anhydrous magnesium sulfate, and concentrated under reduced pressure. The resulting residue was purified by chromatography (silica gel, hexane:ethyl acetate=85:15) to give the title compound (10.97 g).

後処理

  1. washwas washed in turn with 1N hydrochloric acid, saturated aqueous sodium bicarbonate solution and saturated aqueous sodium chloride solution
  2. dry with materialThe solution was dried over anhydrous magnesium sulfate
  3. concentrationconcentrated under reduced pressure
  4. customThe resulting residue was purified by chromatography (silica gel, hexane:ethyl acetate=85:15)

出典と根拠

ORDレコード
ord-405bd573b94d4a1ba7f60b693790c78d
出典データセット
uspto-grants-2008_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07375115B2

反応ノート

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