Hydrochloric Acid → 3,5-Diethyl-4-(4-(2,2-diethoxyethoxy)butyloxy)phenol

HRID 2305065ノート

反応式

HRID 2305065 の反応式
[CH2:1]([C:3]1[CH:4]=[C:5]([O:25]C(=O)C2C=CC=CC=2)[CH:6]=[C:7]([CH2:23][CH3:24])[C:8]=1[O:9][CH2:10][CH2:11][CH2:12][CH2:13][O:14][CH2:15][CH:16]([O:20][CH2:21][CH3:22])[O:17][CH2:18][CH3:19])[CH3:2].[OH-].[K+].Cl>CO.O>[CH2:23]([C:7]1[CH:6]=[C:5]([OH:25])[CH:4]=[C:3]([CH2:1][CH3:2])[C:8]=1[O:9][CH2:10][CH2:11][CH2:12][CH2:13][O:14][CH2:15][CH:16]([O:20][CH2:21][CH3:22])[O:17][CH2:18][CH3:19])[CH3:24]

参加物

6

反応物 3

HCID 313Hydrochloric AcidHCID 14797Potassium HydroxideHCID 184296493,5-Diethyl-1-benzoyloxy-4-(4-(2,2-diethoxyethoxy)butyloxy)benzene

生成物 1

HCID 184295323,5-Diethyl-4-(4-(2,2-diethoxyethoxy)butyloxy)phenol収率 94%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 962Water溶媒

実験手順

To a solution of 31.0 g of 3,5-diethyl-1-benzoyloxy-4-(4-(2,2-diethoxyethoxy)butyloxy)benzene dissolved in 100 ml of methanol was added a solution of 5.1 g of potassium hydroxide dissolved in 25 g of water. After stirring at room temperature for 1 hour, the reaction mixture was acidified by the addition of diluted hydrochloric acid, and concentrated. The residue was poured into water, and extracted twice with ethyl acetate. The ethyl acetate layers were combined, washed with water, dried over anhydrous magnesium sulfate, and concentrated to give a crude product. This crude product was subjected to silica gel chromatography, which afforded 0.60 g (yield, 94%) of 3,5-diethyl-4-(4-(2,2-diethoxyethoxy)butyloxy)phenol, nD25.0 1.4890.

後処理

  1. concentrationconcentrated
  2. additionThe residue was poured into water
  3. extractionextracted twice with ethyl acetate
  4. washwashed with water
  5. dry with materialdried over anhydrous magnesium sulfate
  6. concentrationconcentrated
  7. customto give a crude product

出典と根拠

ORDレコード
ord-da694d7a23c14604a437420810a7eae0
出典データセット
uspto-grants-2002_08
特許番号
US06437184B1

反応ノート

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