Potassium Iodide → HCID 68154186、化合物

HRID 341030

反応式

HRID 341030 の反応式
[O:1]=[C:2]1[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[NH:5][CH:4]=[C:3]1[C:12]([O:14][CH2:15][CH3:16])=[O:13].Br[CH2:18][C:19]1[CH:24]=[CH:23][C:22]([C:25]2[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=2)=[CH:21][CH:20]=1.[I-].[K+].C(=O)([O-])[O-].[K+].[K+]>CN(C)C=O.C(OCC)(=O)C.O>[C:22]1([C:25]2[CH:26]=[CH:27][CH:28]=[CH:29][CH:30]=2)[CH:21]=[CH:20][C:19]([CH2:18][N:5]2[C:6]3[C:11](=[CH:10][CH:9]=[CH:8][CH:7]=3)[C:2](=[O:1])[C:3]([C:12]([O:14][CH2:15][CH3:16])=[O:13])=[CH:4]2)=[CH:24][CH:23]=1

参加物

8

反応物 4

HCID 4875Potassium IodideHCID 11430Potassium CarbonateHCID 220876Ethyl 4-oxo-1,4-dihydroquinoline-3-carboxylateHCID 2577161,1'-Biphenyl, 4-(bromomethyl)-

生成物 1

HCID 68154186HCID 68154186、化合物

試薬・触媒・溶媒 3

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒HCID 8857Ethyl Acetate溶媒

実験手順

Ethyl 4-oxo-1,4-dihydroquinoline-3-carboxylate (6.11 g, 28.1 mmol), 4-(bromomethyl)biphenyl (9.04 g, 36.6 mmol, 1.3 equiv), potassium iodide (467 mg, 2.81 mmol, 0.1 equiv) and potassium carbonate (9.72 g, 70.3 mmol, 2.5 equiv) were combined in N,N-dimethylformamide (10 mL) and stirred at ambient temperature for 18 hours. The mixture was poured into water (100 mL) and ethyl acetate (100 mL) and aged for 2 hours. The mixture was filtered, the filtrate discarded and the solid was dissolved in dichloromethane (100 mL), dried with sodium sulfate, filtered and concentrated in vacuo, providing the titled compound.

後処理

  1. waitaged for 2 hours
  2. filtrationThe mixture was filtered
  3. dissolutionthe solid was dissolved in dichloromethane (100 mL)
  4. dry with materialdried with sodium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-1a23ca74b2bf44d48316ae4eece1fb81
出典データセット
uspto-grants-2014_11
特許番号
US08895580B2

関連ノート

読み込み中…