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N-Iodosuccinimide → 7-Iodo-5-methylimidazo[5,1-b]thiazole

HRID 1839304
ノート
印刷プレビュー

反応式

HRID 1839304 の反応式
[CH3:1][C:2]1[N:9]2[C:5]([S:6][CH:7]=[CH:8]2)=[CH:4][N:3]=1.[I:10]N1C(=O)CCC1=O>ClCCl.IN1C(=O)CCC1=O>[I:10][C:4]1[N:3]=[C:2]([CH3:1])[N:9]2[CH:8]=[CH:7][S:6][C:5]=12
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 2

HCID 120273N-IodosuccinimideHCID 177738035-Methylimidazo[5,1-b]thiazole

生成物 1

HCID 226318267-Iodo-5-methylimidazo[5,1-b]thiazole収率 105.1%

試薬・触媒・溶媒 2

HCID 120273N-Iodosuccinimide触媒HCID 6344Dichloromethane溶媒

実験手順

5-Methylimidazo[5,1-b]thiazole (6.90 g) was dissolved in 500 ml of dichloromethane. N-Iodosuccinimide (10.6 g) was added to the solution. The mixture was stirred at room temperature for 24 hr. N-Iodosuccinimide (1.06 g) was added thereto, followed by stirring for additional one hr. The reaction solution was washed with an aqueous sodium thiosulfate solution and brine in that order, dried over anhydrous magnesium sulfate, and then filtered. The solvent was removed by distillation under the reduced pressure. The residue was dissolved in 200 ml of dichloromethane and 100 ml of ethyl acetate. Silica gel (30 g) was added to the solution. The mixture was stirred. The silica gel was removed by filtration. The filtrate was washed with 200 ml of a mixed solution of dichloromethane:ethyl acetate=2:1. The filtrate was concentrated under the reduced pressure to give 13.08 g of 7-iodo-5-methylimidazo[5,1-b]thiazole.

後処理

  1. stirringby stirring for additional one hr
  2. washThe reaction solution was washed with an aqueous sodium thiosulfate solution and brine in that order
  3. dry with materialdried over anhydrous magnesium sulfate
  4. filtrationfiltered
  5. customThe solvent was removed by distillation under the reduced pressure
  6. dissolutionThe residue was dissolved in 200 ml of dichloromethane
  7. additionSilica gel (30 g) was added to the solution
  8. stirringThe mixture was stirred
  9. customThe silica gel was removed by filtration
  10. washThe filtrate was washed with 200 ml of a mixed solution of dichloromethane
  11. concentrationThe filtrate was concentrated under the reduced pressure

出典と根拠

ORDレコード
ord-59036cf0891f4f4bb8688adad5b5c976
出典データセット
uspto-grants-2004_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06677331B2

反応ノート

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