Sodium Iodide → 3-(2-Cyanophenyl)-5-(2-pyridyl)-2(1H)-pyridone

HRID 229657노트

반응식

HRID 229657 반응식
Cl[Si](C)(C)C.[C:6]([C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][C:9]=1[C:14]1[C:15]([O:26]C)=[N:16][CH:17]=[C:18]([C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][N:21]=2)[CH:19]=1)#[N:7].[I-].[Na+].C(=O)(O)[O-].[Na+]>C(#N)C>[C:6]([C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][C:9]=1[C:14]1[C:15](=[O:26])[NH:16][CH:17]=[C:18]([C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][N:21]=2)[CH:19]=1)#[N:7]

참가 물질

6

반응물 4

HCID 5238Sodium IodideHCID 6397ChlorotrimethylsilaneHCID 516892Sodium BicarbonateHCID 223190893-(2-Cyanophenyl)-5-(2-pyridyl)-2-methoxypyridine

생성물 1

HCID 223189453-(2-Cyanophenyl)-5-(2-pyridyl)-2(1H)-pyridone수율 57.8%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

Chlorotrimethylsilane (0.1 ml) was added to a suspension of 0.20 g of 3-(2-cyanophenyl)-5-(2-pyridyl)-2-methoxypyridine and 0.12 g of sodium iodide in 10 ml of acetonitrile and the mixture was stirred at room temperature for 3 hours. A saturated sodium bicarbonate solution was added to the mixture followed by extracting with ethyl acetate. The ethyl acetate layer was washed with water and a saturated saline solution and dried over magnesium sulfate. The solvent was concentrated in vacuo and the residue was purified by a silica gel column chromatography (ethyl acetate:hexane=1:1) to give 0.11 g of the title compound in pale yellow powder.

후처리

  1. extractionby extracting with ethyl acetate
  2. washThe ethyl acetate layer was washed with water
  3. dry with materiala saturated saline solution and dried over magnesium sulfate
  4. concentrationThe solvent was concentrated in vacuo
  5. customthe residue was purified by a silica gel column chromatography (ethyl acetate:hexane=1:1)

출처 및 근거

ORD 기록
ord-c1166e3b660d48e5b6f263e265c9facd
출처 데이터셋
uspto-grants-2009_07
특허 번호
US07563811B2

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