Dimethylformamide → 4-iodo-N-methyl-2-nitroaniline

HRID 2273321노트

반응식

HRID 2273321 반응식
[I:1][C:2]1[CH:7]=[CH:6][C:5]([NH2:8])=[C:4]([N+:9]([O-:11])=[O:10])[CH:3]=1.[H-].[Na+].[CH3:14]N(C=O)C.IC>O>[I:1][C:2]1[CH:7]=[CH:6][C:5]([NH:8][CH3:14])=[C:4]([N+:9]([O-:11])=[O:10])[CH:3]=1

참가 물질

6

반응물 4

HCID 6228DimethylformamideHCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 113690724-Iodo-2-nitroaniline

생성물 1

HCID 658098494-iodo-N-methyl-2-nitroaniline

시약·촉매·용매 1

HCID 962Water용매

실험 절차

To a mixture of 4-iodo-2-nitro-phenyl amine (2.0 g), 60% sodium hydride (oil) (330 mg), and DMF (20 ml) was added dropwise iodomethane (470 μL) while ice-cooling. The reaction mixture was heasted to room temperature, and then stirred for 2 hours. To the reaction mixture was added water, and the mixture was extracted with ethyl acetate. The organic layer was dried over sodium sulfate, and concentrated under reduced pressure. The residue was subjected to silica gel column chromatography to give (4-iodo-2-nitro-phenyl)-methyl-amine (2.0 g).

후처리

  1. temperaturecooling
  2. customwas heasted to room temperature
  3. extractionthe mixture was extracted with ethyl acetate
  4. dry with materialThe organic layer was dried over sodium sulfate
  5. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-e8255826b1ce4047863a4e03d65b57a5
출처 데이터셋
uspto-grants-2015_09
특허 번호
US09120823B2

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