Cesium carbonate → HCID 19864853, 화합물

HRID 1200256노트

반응식

HRID 1200256 반응식
[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

참가 물질

6

반응물 3

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

생성물 1

HCID 19864853HCID 19864853, 화합물수율 74%

시약·촉매·용매 2

HCID 4875Potassium Iodide촉매HCID 180Acetone용매

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-3dcfdd0f16e14ffb833bea4784816fe0
출처 데이터셋
uspto-grants-1990_02
특허 번호
US04904786

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