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

HRID 1092861ノート

反応式

HRID 1092861 の反応式
[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

参加物

7

反応物 4

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

生成物 1

HCID 166551311-Methoxymethyl-2-bromo-4-nitroimidazole収率 86.9%

試薬・触媒・溶媒 2

HCID 962Water溶媒2 回HCID 8857Ethyl Acetate溶媒

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-cc45c9dceb3f499396d4926808a11a56
出典データセット
uspto-grants-2012_03
特許番号
US08129544B2

反応ノート

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