Potassium Carbonate → HCID 66822369, 화합물

HRID 2406572

반응식

HRID 2406572 반응식
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]

참가 물질

6

반응물 3

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

생성물 1

HCID 66822369HCID 66822369, 화합물수율 98.8%

시약·촉매·용매 2

HCID 180Acetone용매HCID 8857Ethyl Acetate용매

실험 절차

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)+.

후처리

  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

출처 및 근거

ORD 기록
ord-e46f2f20693e44b7b8d6e43fb387b48a
출처 데이터셋
uspto-grants-2014_08
특허 번호
US08809377B2

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