Triethylamine → Imidazo[1,2-a]pyridine,5-[(4-chlorobutyl)thio]-

HRID 357000

反応式

HRID 357000 の反応式
Br[CH2:2][CH2:3][CH2:4][CH2:5][Cl:6].[SH:7][C:8]1[N:13]2[CH:14]=[CH:15][N:16]=[C:12]2[CH:11]=[CH:10][CH:9]=1.C(N(CC)CC)C>C(O)C>[Cl:6][CH2:5][CH2:4][CH2:3][CH2:2][S:7][C:8]1[N:13]2[CH:14]=[CH:15][N:16]=[C:12]2[CH:11]=[CH:10][CH:9]=1

参加物

5

実験手順

In a nitrogen atmosphere, 8.87 ml (77 mmol) of 1-bromo-4-chlorobutane was added to a solution of 10.51 g (70 mmol) of 5-mercaptoimidazo[1,2-a]pyridine and 10.73 ml (77 mmol) of triethylamine in 150 ml of ethanol was added, followed by stirring at room temperature for 16 hours. After the solvent was distilled off, the residue was dissolved in dichloromethane. This solution was washed with saturated aqueous sodium hydrogen carbonate and dried, after which the solvent was distilled off. The residue was purified by column chromatography (eluent: ethyl acetate) to yield 12.93 g (76.7%, light brown oily substance) of the desired product.

後処理

  1. additionwas added
  2. distillationAfter the solvent was distilled off
  3. dissolutionthe residue was dissolved in dichloromethane
  4. washThis solution was washed with saturated aqueous sodium hydrogen carbonate
  5. customdried
  6. distillationafter which the solvent was distilled off
  7. customThe residue was purified by column chromatography (eluent: ethyl acetate)

出典と根拠

ORDレコード
ord-afc7370ad75e49a9ac250316b96f5076
出典データセット
uspto-grants-1998_11
特許番号
US05840732

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