Cesium carbonate → HCID 19864853、化合物

HRID 1200256ノート

反応式

HRID 1200256 の反応式
[O:1]1[CH2:5][CH2:4][O:3][CH:2]1[C:6]1[CH:11]=[CH:10][CH:9]=[C:8]([OH:12])[CH:7]=1.Cl[CH2:14][C:15]1[CH:24]=[CH:23][C:22]2[C:17](=[CH:18][CH:19]=[CH:20][CH:21]=2)[N:16]=1.C(=O)([O-])[O-].[Cs+].[Cs+]>CC(C)=O.[I-].[K+]>[O:1]1[CH2:5][CH2:4][O:3][CH:2]1[C:6]1[CH:7]=[C:8]([CH:9]=[CH:10][CH:11]=1)[O:12][CH2:14][C:15]1[CH:24]=[CH:23][C:22]2[C:17](=[CH:18][CH:19]=[CH:20][CH:21]=2)[N:16]=1

参加物

6

反応物 3

HCID 10796Cesium carbonateHCID 203942-(Chloromethyl)quinolineHCID 132801193-(1,3-Dioxolan-2-yl)phenol

生成物 1

HCID 19864853HCID 19864853、化合物収率 74%

試薬・触媒・溶媒 2

HCID 4875Potassium Iodide触媒HCID 180Acetone溶媒

実験手順

A solution of the ketal of Step A, above, (10 g, 0.06 mol), 2-chloromethylquinoline (10.6 g, 0.06 mol), cesium carbonate (20.0 g, 0.06 mol) and potassium iodide (0.16 g, 0.001 mol) in 250 ml acetone is refluxed 20 hours. The solution is filtered through Celite and silica gel and the solvent is removed in vacuo. The resulting crude solid is recrystallized using 2-propanol to give 13.7 g of crystalline solid (74% yield) m.p. 67°-69° C.

後処理

  1. filtrationThe solution is filtered through Celite and silica gel
  2. customthe solvent is removed in vacuo
  3. customThe resulting crude solid is recrystallized

出典と根拠

ORDレコード
ord-3dcfdd0f16e14ffb833bea4784816fe0
出典データセット
uspto-grants-1990_02
特許番号
US04904786

反応ノート

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