Potassium Carbonate → HCID 66822369、化合物

HRID 2406572

反応式

HRID 2406572 の反応式
Cl.[CH2:2]([N:4]([CH2:8][CH3:9])[CH2:5][CH2:6]Cl)[CH3:3].[OH:10][C:11]1[CH:16]=[CH:15][C:14]([C:17](=[O:21])[CH2:18][CH2:19][CH3:20])=[CH:13][CH:12]=1.C(=O)([O-])[O-].[K+].[K+]>CC(C)=O.C(OCC)(=O)C>[CH2:2]([N:4]([CH2:8][CH3:9])[CH2:5][CH2:6][O:10][C:11]1[CH:12]=[CH:13][C:14]([C:17](=[O:21])[CH2:18][CH2:19][CH3:20])=[CH:15][CH:16]=1)[CH3:3]

参加物

6

反応物 3

HCID 11430Potassium CarbonateHCID 133631-Chloro-2-(diethylamine)ethane hydrochlorideHCID 660921-Butanone, 1-(4-hydroxyphenyl)-

生成物 1

HCID 66822369HCID 66822369、化合物収率 98.8%

試薬・触媒・溶媒 2

HCID 180Acetone溶媒HCID 8857Ethyl Acetate溶媒

実験手順

2-(Diethylamino)ethyl chloride hydrochloride (624 mg, 3.65 mmol) was added to a stirred solution of p-hydroxybutyrophenone (200 mg, 1.21 mmol) in anhydrous acetone (6 mL) followed by the addition of potassium carbonate (668 mg, 4.84 mmol). The resulting mixture was heated at reflux for 48 hours. The mixture was diluted with ethyl acetate, washed with water (2×) and sat. brine, dried over sodium sulfate, and concentrated to an oil. Flash silica gel column chromatography, eluting with 1:1 hexanes/ethyl acetate, afforded 21 (315 mg, 98%) as a light yellow oil: MS (ES+) m/z 264.1 (M+H)+.

後処理

  1. temperatureThe resulting mixture was heated
  2. temperatureat reflux for 48 hours
  3. washwashed with water (2×) and sat. brine
  4. dry with materialdried over sodium sulfate
  5. concentrationconcentrated to an oil
  6. washFlash silica gel column chromatography, eluting with 1:1 hexanes/ethyl acetate

出典と根拠

ORDレコード
ord-e46f2f20693e44b7b8d6e43fb387b48a
出典データセット
uspto-grants-2014_08
特許番号
US08809377B2

関連ノート

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