Water → 4-Bromo-3-methylbenzene-1,2-diamine

HRID 1429211노트

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HRID 1429211 반응식
[Br:1][C:2]1[C:3]([CH3:12])=[C:4]([C:6]([N+:9]([O-])=O)=[CH:7][CH:8]=1)[NH2:5].[Sn](Cl)Cl.O.[OH-].[Na+]>CCO>[Br:1][C:2]1[C:3]([CH3:12])=[C:4]([NH2:5])[C:6]([NH2:9])=[CH:7][CH:8]=1

참가 물질

6

반응물 4

HCID 962WaterHCID 14798Sodium HydroxideHCID 24479Stannous ChlorideHCID 666306133-Bromo-2-methyl-6-nitroaniline

생성물 1

HCID 592142734-Bromo-3-methylbenzene-1,2-diamine수율 88%

시약·촉매·용매 1

HCID 702Ethanol용매

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온도
70 °C

실험 절차

To a solution of 3-bromo-2-methyl-6-nitroaniline (0.45 g, 1.95 mmol) in EtOH (6 mL) was added tin(II) chloride (1.48 g, 7.8 mmol), and the resulting solution was stirred at 70° C. for 4 hours. The mixture was cooled to room temperature and poured into water, and 1 N aq. NaOH was added to adjust to pH>7. The resulting mixture was extracted with CH2Cl2 (2×), and the combined extracts were dried over Na2SO4. The drying agent was filtered off and solvent was removed in vacuo to give the title compound as an oil (0.34 g, 88%).

후처리

  1. temperatureThe mixture was cooled to room temperature
  2. additionwas added
  3. extractionThe resulting mixture was extracted with CH2Cl2 (2×)
  4. dry with materialthe combined extracts were dried over Na2SO4
  5. filtrationThe drying agent was filtered off
  6. customsolvent was removed in vacuo

출처 및 근거

ORD 기록
ord-77c541f335974d7a94c18a46ed4354b9
출처 데이터셋
uspto-grants-2015_01
특허 번호
US08937150B2

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