Water → HCID 66761312、化合物

HRID 876315ノート

反応式

HRID 876315 の反応式
[F:1][C:2]([F:26])([F:25])[O:3][C:4]1[CH:9]=[CH:8][C:7]([CH:10]2[CH2:15][NH:14][CH2:13][CH:12]([NH:16][C:17](=[O:24])[C:18]3[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=3)[CH2:11]2)=[CH:6][CH:5]=1.[CH3:27][N:28]1[CH2:33][CH2:32][N:31]([C:34](Cl)=[O:35])[CH2:30][CH2:29]1.C(N(CC)CC)C.O>ClCCl>[CH3:27][N:28]1[CH2:33][CH2:32][N:31]([C:34]([N:14]2[CH2:15][CH:10]([C:7]3[CH:6]=[CH:5][C:4]([O:3][C:2]([F:1])([F:25])[F:26])=[CH:9][CH:8]=3)[CH2:11][CH:12]([NH:16][C:17]([C:18]3[CH:19]=[CH:20][CH:21]=[CH:22][CH:23]=3)=[O:24])[CH2:13]2)=[O:35])[CH2:30][CH2:29]1

参加物

6

反応物 4

HCID 962WaterHCID 8471TriethylamineHCID 30169354-Methyl-1-piperazinecarbonyl chlorideHCID 66701272N-{5-[4-(trifluoromethoxy)phenyl]piperidin-3-yl}benzamide

生成物 1

HCID 66761312HCID 66761312、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

At 0° C., 100 mg (0.27 mmol) of N-{5-[4-(trifluoromethoxy)phenyl]piperidin-3-yl}benzamide were initially charged in 1.5 ml of dichloromethane, and 89 mg (0.55 mmol) of 4-methylpiperazine-1-carbonyl chloride and 58 μl (0.412 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: 104 mg (77% 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-1cabfb216ec04ea1acd54e5d828f0ac4
出典データセット
uspto-grants-2015_03
特許番号
US08987248B2

反応ノート

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