N-Iodosuccinimide → HCID 23449208、化合物

HRID 1839331ノート

反応式

HRID 1839331 の反応式
[I:1]N1C(=O)CCC1=O.[CH3:9][S:10][C:11]1[N:12]=[CH:13][N:14]2[CH:18]=[CH:17][S:16][C:15]=12>ClCCl.[Cl-].[Na+].O>[I:1][C:13]1[N:14]2[C:15]([S:16][CH:17]=[CH:18]2)=[C:11]([S:10][CH3:9])[N:12]=1

参加物

5

反応物 2

HCID 120273N-IodosuccinimideHCID 226315297-Methylthioimidazo[5,1-b]thiazole

生成物 1

HCID 23449208HCID 23449208、化合物収率 95.3%

試薬・触媒・溶媒 2

HCID 6344Dichloromethane溶媒HCID 57417360Sodium chloride; water溶媒

実験手順

N-Iodosuccinimide (3.08 g) was added under ice cooling to a solution of 2.28 g of 7-methylthioimidazo[5,1-b]thiazole in dichloromethane. The mixture was stirred at room temperature for 7 hr. Saturated brine was added to the reaction mixture, followed by separation. The organic layer was washed with a dilute aqueous sodium thiosulfate solution and saturated brine in that order, and then dried over anhydrous magnesium sulfate. The solvent was removed by distillation. The residue was purified by column chromatography on silica gel (ethyl acetate:dichloromethane=1:1) to give 3.78 g of 5-iodo-7-methylthioimidazo[5,1-b]thiazole.

後処理

  1. customfollowed by separation
  2. washThe organic layer was washed with a dilute aqueous sodium thiosulfate solution and saturated brine in that order
  3. dry with materialdried over anhydrous magnesium sulfate
  4. customThe solvent was removed by distillation
  5. customThe residue was purified by column chromatography on silica gel (ethyl acetate:dichloromethane=1:1)

出典と根拠

ORDレコード
ord-1ac3c463b3684cecb09c58d033233cac
出典データセット
uspto-grants-2004_01
特許番号
US06677331B2

反応ノート

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