N-Iodosuccinimide → HCID 23449208, 화합물

HRID 989866노트

반응식

HRID 989866 반응식
[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

참가 물질

5

반응물 2

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

생성물 1

HCID 23449208HCID 23449208, 화합물수율 95.3%

시약·촉매·용매 2

HCID 6344Dichloromethane용매HCID 57417360Sodium chloride; water용매

실험 절차

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 for7 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.

후처리

  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)

출처 및 근거

ORD 기록
ord-e67d6905fb164985ace5c850496c8311
출처 데이터셋
uspto-grants-2002_10
특허 번호
US06458780B1

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