Sodium Iodide → HCID 57722476, 화합물

HRID 1931223노트

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HRID 1931223 반응식
[I-].[Na+].Cl[Si](C)(C)[CH3:5].[CH2:8]([O:15][C:16]1[C:21]([C:22](=[O:32])[NH:23][CH2:24][C:25]2[CH:30]=[CH:29][C:28]([F:31])=[CH:27][CH:26]=2)=[CH:20][N:19]=[C:18]([C:33]([O:35][CH3:36])=[O:34])[C:17]=1[O:37][CH3:38])[C:9]1C=CC=CC=1.S([O-])(O)=O.[Na+]>C(#N)C>[CH3:17][C:16]([CH3:21])=[O:15].[CH:16]([O:15][CH:8]([CH3:9])[CH3:5])([CH3:17])[CH3:21].[F:31][C:28]1[CH:27]=[CH:26][C:25]([CH2:24][NH:23][C:22]([C:21]2[C:16](=[O:15])[C:17]([O:37][CH3:38])=[C:18]([C:33]([O:35][CH3:36])=[O:34])[NH:19][CH:20]=2)=[O:32])=[CH:30][CH:29]=1

참가 물질

7

반응물 4

HCID 5238Sodium IodideHCID 6397ChlorotrimethylsilaneHCID 23665763Sodium BisulfiteHCID 57722482HCID 57722482, 화합물

생성물 2

HCID 22221350Acetone diisopropyl etherHCID 57722476HCID 57722476, 화합물수율 253.3%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

To a suspension of sodium iodide (5.51 g, 36.8 mmol) in acetonitrile (50 ml) was added chlorotrimethylsilane (4.66 ml, 36.8 mmol), and the mixture was stirred at room temperature for 10 minutes. After to this solution was added the compound 27 (2.60 g, 6.13 mmol) under ice-cooling, this was stirred at the same temperature for 20 minutes. To the reaction solution was added a 5% sodium hydrogen sulfite solution, followed by extraction with ethyl acetate. The extract was washed with an aqueous saturated sodium bicarbonate solution and an aqueous saturated sodium chlorite solution, and dried with anhydrous sodium sulfate. The solvent was distilled off under reduced pressure, and the resulting solid matter was recrystallized to obtain (acetone-diisopropyl ether) and methyl 5-(4-fluorobenzylcarbamoyl)-3-methoxy-4-oxo-1,4-dihydropyridine-2-carboxylate 28 (1.73 g, 84%) as a colorless crystal.

후처리

  1. temperaturecooling
  2. stirringthis was stirred at the same temperature for 20 minutes
  3. extractionfollowed by extraction with ethyl acetate
  4. washThe extract was washed with an aqueous saturated sodium bicarbonate solution
  5. dry with materialan aqueous saturated sodium chlorite solution, and dried with anhydrous sodium sulfate
  6. distillationThe solvent was distilled off under reduced pressure
  7. customthe resulting solid matter was recrystallized

출처 및 근거

ORD 기록
ord-f5152a464b7246fb8827c0efaa685fbd
출처 데이터셋
uspto-grants-2012_05
특허 번호
US08188271B2

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