Methyl iodide → N-BOC-N-Methyl-3-bromoaniline

HRID 1092274

반응식

HRID 1092274 반응식
[Br:1][C:2]1[CH:3]=[C:4]([NH:8][C:9](=[O:15])[O:10][C:11]([CH3:14])([CH3:13])[CH3:12])[CH:5]=[CH:6][CH:7]=1.[H-].[Na+].[CH3:18]I>CN(C=O)C>[Br:1][C:2]1[CH:3]=[C:4]([N:8]([CH3:18])[C:9](=[O:15])[O:10][C:11]([CH3:12])([CH3:14])[CH3:13])[CH:5]=[CH:6][CH:7]=1

참가 물질

5

반응물 3

HCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 2757254N-(tert-Butoxycarbonyl)-3-bromoaniline

생성물 1

HCID 22997148N-BOC-N-Methyl-3-bromoaniline수율 95%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

To a solution of 114 g (447 mmol) of tert-butyl (3-bromophenyl)carbamate in 800 ml of DMF are added portionwise 19 g (475 mmol) of sodium hydride (60% in oil) and the reaction medium is stirred until the evolution of gas has ceased. 29.3 ml (470 mmol) of methyl iodide are added dropwise and stirring is continued for 18 hours. The reaction medium is poured into ice-water and extracted with ethyl acetate. The organic phase is separated out by settling of the phases, dried over magnesium sulfate and evaporated. 115 g of tert-butyl (3-bromophenyl)-N-methylcarbamate are obtained in a yield of 95%.

후처리

  1. stirringstirring
  2. extractionextracted with ethyl acetate
  3. customThe organic phase is separated out
  4. dry with materialdried over magnesium sulfate
  5. customevaporated

출처 및 근거

ORD 기록
ord-ba3433e1390b426396c07058c5da4ea4
출처 데이터셋
uspto-grants-2012_03
특허 번호
US08129416B2

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