2-Methylimidazole → HCID 14207213、化合物

HRID 1647736ノート

反応式

HRID 1647736 の反応式
Br[CH2:2][CH2:3][CH2:4][O:5][C:6]1[CH:7]=[C:8]2[C:13](=[CH:14][CH:15]=1)[NH:12][C:11](=[O:16])[CH2:10][CH2:9]2.[CH3:17][C:18]1[NH:19][CH:20]=[CH:21][N:22]=1.C1CCN2C(=NCCC2)CC1>C(O)(C)C>[CH3:17][C:18]1[N:19]([CH2:2][CH2:3][CH2:4][O:5][C:6]2[CH:7]=[C:8]3[C:13](=[CH:14][CH:15]=2)[NH:12][C:11](=[O:16])[CH2:10][CH2:9]3)[CH:20]=[CH:21][N:22]=1

参加物

5

反応物 3

HCID 127492-MethylimidazoleHCID 811841,8-Diazabicyclo(5.4.0)undec-7-eneHCID 13055728HCID 13055728、化合物

生成物 1

HCID 14207213HCID 14207213、化合物

試薬・触媒・溶媒 1

HCID 3776Isopropanol溶媒

実験手順

2.0 Grams (7.0 mM) of 6-(3-bromopropoxy)-3,4-dihydrocarbostyril, 2.2 g (7.7 mM) of 2-methylimidazol and 1.3 ml (8.4 mM) of DBU were dissolved in 80 ml of isopropanol, and the resulting solution was refluxed by heating for 20 hours. The reaction mixture was concentrated, and to the resulting residue was added water, then extracted with chloroform. The chloroform extract was washed with water, dried with anhydrous sodium sulfate, then concentrated. The resulting residue was purified by means of a silica gel column chromatography (eluent: dichloromethane: methanol=20:1), and recrystallized from ethanol-n-hexane to yield 1.0 g of 6- [3-(2-methyl-1-imidazolyl)propoxy]-3,4-dihydrocarbostyril. White powdery substance. Melting point: 141.5°-142.5° C.

後処理

  1. temperaturethe resulting solution was refluxed
  2. temperatureby heating for 20 hours
  3. concentrationThe reaction mixture was concentrated
  4. additionto the resulting residue was added water
  5. extractionextracted with chloroform
  6. extractionThe chloroform extract
  7. washwas washed with water
  8. dry with materialdried with anhydrous sodium sulfate
  9. concentrationconcentrated
  10. customThe resulting residue was purified by means of a silica gel column chromatography (eluent: dichloromethane: methanol=20:1)
  11. customrecrystallized from ethanol-n-hexane

出典と根拠

ORDレコード
ord-42a55886a8b94f6b97ff53d66eb228c2
出典データセット
uspto-grants-1995_07
特許番号
US05434164

反応ノート

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