Dimethylformamide → 1-Methoxymethyl-2-bromo-4-nitroimidazole

HRID 2221384노트

반응식

HRID 2221384 반응식
[Br:1][C:2]1[N:3]([CH2:11][O:12][CH3:13])[C:4](Br)=[C:5]([N+:7]([O-:9])=[O:8])[N:6]=1.S([O-])([O-])=O.[Na+].[Na+].CN(C)C=O.C(=O)([O-])O.[Na+]>O.C(OCC)(=O)C>[Br:1][C:2]1[N:3]([CH2:11][O:12][CH3:13])[CH:4]=[C:5]([N+:7]([O-:9])=[O:8])[N:6]=1

참가 물질

7

반응물 4

HCID 6228DimethylformamideHCID 24437Sodium SulfiteHCID 516892Sodium BicarbonateHCID 5422602,5-Dibromo-1-methoxymethyl-4-nitroimidazole

생성물 1

HCID 166551311-Methoxymethyl-2-bromo-4-nitroimidazole수율 86.9%

시약·촉매·용매 2

HCID 962Water용매2회HCID 8857Ethyl Acetate용매

실험 절차

Suspension of 2,5-dibromo-1-methoxymethyl-4-nitroimidazole (17.15 g), sodium sulfite (13.73 g), dimethylformamide (100 ml) and water (50 ml) was stirred at a room temperature for 8 hours. The reaction mixture was neutralized with an aqueous solution being saturated with sodium hydrogencarbonate, then ethyl acetate and water were added. The organic layer was washed with an aqueous solution being saturated with sodium chloride, and dried over anhydrous sodium sulfate, then concentrated under a reduced pressure to obtain 2-bromo-1-methoxymethyl-4-nitroimidazole (11.17 g, yield: 86.8%) of white powdery product.

후처리

  1. washThe organic layer was washed with an aqueous solution
  2. dry with materialdried over anhydrous sodium sulfate
  3. concentrationconcentrated under a reduced pressure

출처 및 근거

ORD 기록
ord-862729e1b62c45468f4360d89380bf94
출처 데이터셋
uspto-grants-2008_05
특허 번호
US07368579B2

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