Potassium Iodide → HCID 13560729, 화합물

HRID 414838노트

반응식

HRID 414838 반응식
Cl.Cl[CH2:3][C:4]1[CH:13]=[CH:12][C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[N:5]=1.[C:14](=[O:17])([O-])[O-].[K+].[K+].[I-].[K+].[C:22](=[O:25])([O-])[O-].[Cs+].[Cs+]>CC(C)=O>[C:22]([C:7]1[CH:6]=[C:14]([CH:10]=[CH:9][CH:8]=1)[O:17][CH2:3][C:4]1[CH:13]=[CH:12][C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[N:5]=1)(=[O:25])[CH2:11][CH2:12][CH2:13][CH2:4][CH3:3]

참가 물질

6

반응물 4

HCID 4875Potassium IodideHCID 10796Cesium carbonateHCID 11430Potassium CarbonateHCID 30838232-(Chloromethyl)quinoline hydrochloride

생성물 1

HCID 13560729HCID 13560729, 화합물

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

This ketone (1.2 g) was refluxed with 2-chloromethylquinoline hydrochloride (1.3 g), potassium carbonate (8.6 g), potassium iodide (0.05 g) and cesium carbonate (0.05 g) in acetone (300 ml) for 24 hours. The reaction mixture was filtered, and the filtrate was concentrated, dissolved in chloroform, and then washed with sodium hydroxide solution (5%), water and brine. After drying this solution over MgSO4, all volatiles were removed. The residue was purified by chromatography on silica gel (25% ethyl acetate in hexanes). The pure desired product was isolated as a tan solid, m.p. 52°-55° C.

후처리

  1. filtrationThe reaction mixture was filtered
  2. concentrationthe filtrate was concentrated
  3. dissolutiondissolved in chloroform
  4. washwashed with sodium hydroxide solution (5%), water and brine
  5. dry with materialAfter drying this solution over MgSO4
  6. customall volatiles were removed
  7. customThe residue was purified by chromatography on silica gel (25% ethyl acetate in hexanes)

출처 및 근거

ORD 기록
ord-676dbe56a74944e5aa184ea58b8ab008
출처 데이터셋
uspto-grants-1988_12
특허 번호
US04794188

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