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

HRID 357000
ノート
印刷プレビュー

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
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 8471TriethylamineHCID 813641-Bromo-4-chlorobutaneHCID 178418687HCID 178418687、化合物

生成物 1

HCID 18936641Imidazo[1,2-a]pyridine,5-[(4-chlorobutyl)thio]-

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

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
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05840732

反応ノート

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