Potassium Iodide → HCID 68154186, 화합물

HRID 341030노트

반응식

HRID 341030 반응식
[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

참가 물질

8

반응물 4

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

생성물 1

HCID 68154186HCID 68154186, 화합물

시약·촉매·용매 3

HCID 962Water용매HCID 6228Dimethylformamide용매HCID 8857Ethyl Acetate용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-1a23ca74b2bf44d48316ae4eece1fb81
출처 데이터셋
uspto-grants-2014_11
특허 번호
US08895580B2

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