Potassium Iodide → HCID 58351061, 화합물

HRID 475719노트

반응식

HRID 475719 반응식
[Br:1][C:2]1[N:7]=[C:6]([O:8][CH3:9])[C:5]([NH:10][CH:11]=[O:12])=[CH:4][CH:3]=1.[I-].[K+].C(=O)([O-])[O-].[Cs+].[Cs+].Cl[CH2:22][C:23](=[O:25])[CH3:24]>CN(C=O)C>[Br:1][C:2]1[N:7]=[C:6]([O:8][CH3:9])[C:5]([N:10]([CH2:22][C:23](=[O:25])[CH3:24])[CH:11]=[O:12])=[CH:4][CH:3]=1

참가 물질

6

반응물 4

HCID 4875Potassium IodideHCID 6571ChloroacetoneHCID 10796Cesium carbonateHCID 71492501N-(6-bromo-2-methoxypyridin-3-yl)formamide

생성물 1

HCID 58351061HCID 58351061, 화합물수율 100%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

To a mixture of N-(6-bromo-2-methoxypyridin-3-yl)formamide (5.69 g, 24.63 mmol), potassium iodide (0.450 g, 2.71 mmol) and cesium carbonate (28.1 g, 86 mmol) in 66 mL of DMF was added 1-chloropropan-2-one (4.90 mL, 61.6 mmol). The reaction mixture was stirred at rt for 3 days. The reaction mixture was poured into icewater and extracted with ethyl acetate. The combined organic extracts were dried over anhydrous magnesium sulfate and filtered. The solvent was removed in vacuum to give N-(6-bromo-2-methoxypyridin-3-yl)-N-(2-oxopropyl)formamide (7.07 g, 24.62 mmol, 100% yield) as brown solid. LC-MS (M+Na)+=310.9.

후처리

  1. additionThe reaction mixture was poured into icewater
  2. extractionextracted with ethyl acetate
  3. dry with materialThe combined organic extracts were dried over anhydrous magnesium sulfate
  4. filtrationfiltered
  5. customThe solvent was removed in vacuum

출처 및 근거

ORD 기록
ord-75212d285d6b49569884e2ad8fda0dcc
출처 데이터셋
uspto-grants-2014_01
특허 번호
US08637525B2

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