Potassium Iodide → HCID 13560729、化合物

HRID 1285489ノート

反応式

HRID 1285489 の反応式
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]

参加物

6

反応物 4

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

生成物 1

HCID 13560729HCID 13560729、化合物

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

This ketone (1.2 g) was refluxed with 2-chloromethyl-quinoline 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, 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.

後処理

  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. customAfter drying
  6. customall volatiles were removed
  7. customThe residue was purified by chromatography on silica gel (25% ethyl acetate in hexanes)

出典と根拠

ORDレコード
ord-dc648a5aa6ed47979e28121576fdf05c
出典データセット
uspto-grants-1986_01
特許番号
US04567184

反応ノート

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