Potassium Carbonate → HCID 66758476、化合物

HRID 556958ノート

反応式

HRID 556958 の反応式
Br[CH2:2][CH2:3][CH:4]=[C:5]1[C:11]2[CH:12]=[CH:13][CH:14]=[N:15][C:10]=2[CH2:9][O:8][C:7]2[CH:16]=[CH:17][C:18]([C:20]([OH:23])([CH3:22])[CH3:21])=[CH:19][C:6]1=2.C(=O)([O-])[O-].[K+].[K+].[Cl:30][C:31]1[CH:36]=[CH:35][C:34]([NH:37][C:38]2([C:44]#[N:45])[CH2:43][CH2:42][NH:41][CH2:40][CH2:39]2)=[CH:33][CH:32]=1>O.C(#N)C.C(OCC)(=O)C>[Cl:30][C:31]1[CH:32]=[CH:33][C:34]([NH:37][C:38]2([C:44]#[N:45])[CH2:43][CH2:42][N:41]([CH2:2][CH2:3][CH:4]=[C:5]3[C:11]4[CH:12]=[CH:13][CH:14]=[N:15][C:10]=4[CH2:9][O:8][C:7]4[CH:16]=[CH:17][C:18]([C:20]([OH:23])([CH3:22])[CH3:21])=[CH:19][C:6]3=4)[CH2:40][CH2:39]2)=[CH:35][CH:36]=1

参加物

7

反応物 3

HCID 11430Potassium CarbonateHCID 23136852HCID 23136852、化合物HCID 666859992-[5-(3-Bromo-propylidene)-5,1 1-dihydro-10-oxa-1-aza-dibenzo[a,d]cyclohepten-7-yl]-propan-2-ol

生成物 1

HCID 66758476HCID 66758476、化合物収率 8%

試薬・触媒・溶媒 3

HCID 962Water溶媒2 回HCID 6342Acetonitrile溶媒HCID 8857Ethyl Acetate溶媒

反応条件

温度
50 °C

実験手順

The title compound was prepared by dissolving 2-[5-(3-Bromo-propylidene)-5,11-dihydro-10-oxa-1-aza-dibenzo[a,d]cyclohepten-7-yl]-propan-2-ol (106.7 mg, 0.285 mmol) in water (4 ml) and acetonitrile (1 ml). To this was added potassium carbonate (82.7 mg, 0.599 mmol) and 4-(4-Chloro-phenylamino)-piperidine-4-carbonitrile (84.0 mg, 0.356 mmol). The reaction was heated to 50° C. and stirred overnight. The next day the reaction was allowed to cool to room temperature and diluted with ethyl acetate and water. The organic layer was washed twice with water, dried over magnesium sulfate, and concentrated under reduced pressure. The crude residue was purified by reverse phase HPLC to give the title compound (11.5 mg, 8% yield, 88% pure by LC/MS).

後処理

  1. customThe title compound was prepared
  2. temperatureto cool to room temperature
  3. washThe organic layer was washed twice with water
  4. dry with materialdried over magnesium sulfate
  5. concentrationconcentrated under reduced pressure
  6. customThe crude residue was purified by reverse phase HPLC

出典と根拠

ORDレコード
ord-5f3dc4118ae34eae842f435b731c5060
出典データセット
uspto-grants-2011_11
特許番号
US08058287B2

反応ノート

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