Water → N-(1-benzoylpiperidin-4-yl)-4-fluorobenzamide

HRID 49789ノート

反応式

HRID 49789 の反応式
[NH:1]1[CH2:6][CH2:5][CH:4]([NH:7][C:8](=[O:16])[C:9]2[CH:14]=[CH:13][C:12]([F:15])=[CH:11][CH:10]=2)[CH2:3][CH2:2]1.N1C=CC=CC=1.[C:23](Cl)(=[O:30])[C:24]1[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1.O>ClCCl>[C:23]([N:1]1[CH2:2][CH2:3][CH:4]([NH:7][C:8](=[O:16])[C:9]2[CH:14]=[CH:13][C:12]([F:15])=[CH:11][CH:10]=2)[CH2:5][CH2:6]1)(=[O:30])[C:24]1[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1

参加物

6

反応物 4

HCID 962WaterHCID 1049PyridineHCID 7412Benzoyl chlorideHCID 47782264-fluoro-N-(piperidin-4-yl)benzamide

生成物 1

HCID 9797409N-(1-benzoylpiperidin-4-yl)-4-fluorobenzamide

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

To a suspension of N-(piperidin-4-yl)-4-fluorobenzamide (0.5 g) in dichloromethane (5 ml) were added pyridine (218 μl), dichloromethane (5 ml) and benzoyl chloride (290 μl) at ambient temperature. After stirring for 3.5 hours, water (5 ml) was poured into the mixture. An organic layer was separated, and washed with water and brine. After drying with magnesium sulfate, the solvents were removed under reduced pressure. A residue was purified by column chromatography (silica gel, toluene:ethyl acetate=1:1 to ethyl acetate). After rinse with diisopropyl ether, N-(1-benzoylpiperidin-4-yl)-4-fluorobenzamide (515 mg) was obtained.

後処理

  1. customAn organic layer was separated
  2. washwashed with water and brine
  3. dry with materialAfter drying with magnesium sulfate
  4. customthe solvents were removed under reduced pressure
  5. customA residue was purified by column chromatography (silica gel, toluene:ethyl acetate=1:1 to ethyl acetate)
  6. washAfter rinse with diisopropyl ether

出典と根拠

ORDレコード
ord-64d0f593fc724881840098bfc8140046
出典データセット
uspto-grants-2004_03
特許番号
US06710043B1

反応ノート

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