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2-Amino-4-methylpyridine → 2-(4'-Chloropropoxy-2'fluorophenyl)-7-methylimidazo[1,2-a]pyridine

HRID 1268676
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HRID 1268676 반응식
Br[CH2:2][C:3]([C:5]1[CH:10]=[CH:9][C:8]([O:11][CH2:12][CH2:13][CH2:14][Cl:15])=[CH:7][C:6]=1[F:16])=O.[NH2:17][C:18]1[CH:23]=[C:22]([CH3:24])[CH:21]=[CH:20][N:19]=1>C(O)C>[Cl:15][CH2:14][CH2:13][CH2:12][O:11][C:8]1[CH:9]=[CH:10][C:5]([C:3]2[N:17]=[C:18]3[CH:23]=[C:22]([CH3:24])[CH:21]=[CH:20][N:19]3[CH:2]=2)=[C:6]([F:16])[CH:7]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 15332-Amino-4-methylpyridineHCID 22015593alpha-Bromo-2'-fluoro-4'-chloropropoxyacetophenone

생성물 1

HCID 220156172-(4'-Chloropropoxy-2'fluorophenyl)-7-methylimidazo[1,2-a]pyridine

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A solution of the product of Step B (1.0 g) and 2-amino-4-picoline (0.357 g) in ethanol (4 mL) was heated at 73° C. for 18 hours. The reaction mixture was cooled to ambient temperature and the solvent evaporated in vacuo. A portion of the residue was purified via silica gel chromatography (ethyl acetate/hexane) directly. The remainder of the residue was dissolved in methanol/dichloromethane and treated with Dowex® 550A basic resin (Aldrich, Milwaukee, Wis.) for 10 minutes. The resin was removed via filtration and the filtrate evaporated prior to silica gel chromatography (ethyl acetate/hexane). The combined material (0.42 g) containing the title compound was used without further purification.

후처리

  1. customthe solvent evaporated in vacuo
  2. customA portion of the residue was purified via silica gel chromatography (ethyl acetate/hexane) directly
  3. dissolutionThe remainder of the residue was dissolved in methanol/dichloromethane
  4. additiontreated with Dowex® 550A basic resin (Aldrich, Milwaukee, Wis.) for 10 minutes
  5. customThe resin was removed via filtration
  6. customthe filtrate evaporated
  7. additionThe combined material (0.42 g) containing the title compound
  8. customwas used without further purification

출처 및 근거

ORD 기록
ord-dff56547f0fd43f18758f1f979a7febc
출처 데이터셋
uspto-grants-2007_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07199117B2

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