Water → N-{1-(Morpholin-4-ylcarbonyl)-5-[4-(trifluoromethyl)phenyl]piperidin-3-yl}benzenecarboxamide

HRID 876324

反応式

HRID 876324 の反応式
[F:1][C:2]([F:25])([F:24])[C:3]1[CH:8]=[CH:7][C:6]([CH:9]2[CH2:14][NH:13][CH2:12][CH:11]([NH:15][C:16](=[O:23])[C:17]3[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=3)[CH2:10]2)=[CH:5][CH:4]=1.[N:26]1([C:32](Cl)=[O:33])[CH2:31][CH2:30][O:29][CH2:28][CH2:27]1.C(N(CC)CC)C.O>ClCCl>[N:26]1([C:32]([N:13]2[CH2:14][CH:9]([C:6]3[CH:5]=[CH:4][C:3]([C:2]([F:24])([F:1])[F:25])=[CH:8][CH:7]=3)[CH2:10][CH:11]([NH:15][C:16]([C:17]3[CH:18]=[CH:19][CH:20]=[CH:21][CH:22]=3)=[O:23])[CH2:12]2)=[O:33])[CH2:31][CH2:30][O:29][CH2:28][CH2:27]1

参加物

6

反応物 4

HCID 962WaterHCID 8471TriethylamineHCID 848104-Morpholinecarbonyl chlorideHCID 66701397N-{5-[4-(trifluoromethyl)phenyl]piperidin-3-yl}benzamide

生成物 1

HCID 66701371N-{1-(Morpholin-4-ylcarbonyl)-5-[4-(trifluoromethyl)phenyl]piperidin-3-yl}benzenecarboxamide

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

At 0° C., 705 mg (2.02 mmol) of N-{5-[4-(trifluoromethyl)phenyl]piperidin-3-yl}benzamide were initially charged in 70 ml of dichloromethane, and 321 mg (2.02 mmol) of morpholine-4-carbonyl chloride and 564 μl (4.04 mmol) of triethylamine were added. The mixture was slowly warmed to RT overnight. Water was added, and the reaction mixture was extracted. The organic phase was dried over magnesium sulphate and concentrated under reduced pressure. The residue was then purified by preparative HPLC (Reprosil C18, water/acetonitrile gradient). Yield: 960 mg (100% of theory)

後処理

  1. extractionthe reaction mixture was extracted
  2. dry with materialThe organic phase was dried over magnesium sulphate
  3. concentrationconcentrated under reduced pressure
  4. customThe residue was then purified by preparative HPLC (Reprosil C18, water/acetonitrile gradient)

出典と根拠

ORDレコード
ord-358e3ad6b1374a59afa264e74a909f13
出典データセット
uspto-grants-2015_03
特許番号
US08987248B2

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