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

HRID 1268676

반응식

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 물질

4

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
특허 번호
US07199117B2

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