Potassium Carbonate → HCID 66757593、化合物

HRID 917097ノート

反応式

HRID 917097 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2([C:14](=[O:16])[CH3:15])[CH2:13][CH2:12][NH:11][CH2:10][CH2:9]2)=[CH:4][CH:3]=1.C(=O)([O-])[O-].[K+].[K+].Br[CH2:24][CH2:25][CH:26]=[C:27]1[C:33]2[CH:34]=[CH:35][CH:36]=[N:37][C:32]=2[CH2:31][O:30][C:29]2[CH:38]=[CH:39][C:40]([C:42]([OH:45])([CH3:44])[CH3:43])=[CH:41][C:28]1=2>C(#N)C.O>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2([C:14](=[O:16])[CH3:15])[CH2:13][CH2:12][N:11]([CH2:24][CH2:25][CH:26]=[C:27]3[C:33]4[CH:34]=[CH:35][CH:36]=[N:37][C:32]=4[CH2:31][O:30][C:29]4[CH:38]=[CH:39][C:40]([C:42]([OH:45])([CH3:44])[CH3:43])=[CH:41][C:28]3=4)[CH2:10][CH2:9]2)=[CH:4][CH:3]=1

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 231369521-[4-(4-Chloro-phenyl)-piperidin-4-yl]-ethanoneHCID 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 66757593HCID 66757593、化合物

試薬・触媒・溶媒 1

HCID 18373917Acetonitrile--water (1/1)溶媒

実験手順

To a suspension of 1-[4-(4-chloro-phenyl)-piperidin-4-yl]-ethanone in acetonitrile/water (4/1) was added potassium carbonate (221 mg, 1.6 mmol), followed by 2-[5-(3-bromo-propylidene)-5,11-dihydro-10-oxa-1-aza-dibenzo[a,d]cyclohepten-7-yl]-propan-2-ol (150 mg, 0.4 mmol). The reaction mixture was stirred at room temperature for 48 hours and then concentrated in vacuo. The resulting residue was treated with water and extracted with ethyl acetate. Solvent was evaporate from the combined dried (MgSO4) organic extracts. Purification on silica gel chromatography using dichloromethane-methanol (9.5:0.5) afforded the title compound.

後処理

  1. concentrationconcentrated in vacuo
  2. additionThe resulting residue was treated with water
  3. extractionextracted with ethyl acetate
  4. customSolvent was evaporate from the
  5. dry with materialcombined dried (MgSO4) organic extracts
  6. customPurification on silica gel chromatography

出典と根拠

ORDレコード
ord-a502f631654245b5827d9a83614322e1
出典データセット
uspto-grants-2007_09
特許番号
US07271176B2

反応ノート

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