2-Amino-4-methylpyridine → 2-[3-(3-Chloro-propoxy)-phenyl]-7-methyl-imidazo[1,2-a]pyridine

HRID 1268672

反応式

HRID 1268672 の反応式
Br[CH2:2][C:3]([C:5]1[CH:10]=[CH:9][CH:8]=[C:7]([O:11][CH2:12][CH2:13][CH2:14][Cl:15])[CH:6]=1)=O.[NH2:16][C:17]1[CH:22]=[C:21]([CH3:23])[CH:20]=[CH:19][N:18]=1>C(O)C>[Cl:15][CH2:14][CH2:13][CH2:12][O:11][C:7]1[CH:6]=[C:5]([C:3]2[N:16]=[C:17]3[CH:22]=[C:21]([CH3:23])[CH:20]=[CH:19][N:18]3[CH:2]=2)[CH:10]=[CH:9][CH:8]=1

参加物

4

反応物 2

HCID 15332-Amino-4-methylpyridineHCID 220155922-Bromo-1-[3-(3-chloro-propoxy)-phenyl]-ethanone

生成物 1

HCID 220156092-[3-(3-Chloro-propoxy)-phenyl]-7-methyl-imidazo[1,2-a]pyridine収率 48.7%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A solution of the product of Step B (2.6 g) and 2-amino-4-picoline (0.96 g) in ethanol (10 mL) was heated at 73° C. for 2 hours. The reaction mixture was cooled to ambient temperature and the solvent evaporated in vacuo. The residue was dissolved in dichloromethane (75 mL), washed with saturated sodium bicarbonate solution (2×75 mL), brine (75 mL), dried over magnesium sulfate, filtered and evaporated. The residue was purified via silica gel chromatography (ethyl acetate/hexane) to give the title compound (1.3 g).

後処理

  1. customthe solvent evaporated in vacuo
  2. dissolutionThe residue was dissolved in dichloromethane (75 mL)
  3. washwashed with saturated sodium bicarbonate solution (2×75 mL), brine (75 mL)
  4. dry with materialdried over magnesium sulfate
  5. filtrationfiltered
  6. customevaporated
  7. customThe residue was purified via silica gel chromatography (ethyl acetate/hexane)

出典と根拠

ORDレコード
ord-ffb6682226c848c6a12c0079fbbb1746
出典データセット
uspto-grants-2007_04
特許番号
US07199117B2

関連ノート

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