Nitric Acid → 2-Bromo-1,3-dimethyl-4-nitrobenzene

HRID 25272

반응식

HRID 25272 반응식
[N+:1]([O-:4])(O)=[O:2].[Br:5][C:6]1[C:11]([CH3:12])=[CH:10][CH:9]=[CH:8][C:7]=1[CH3:13]>C(O)(=O)C>[CH3:13][C:7]1[C:8]([N+:1]([O-:4])=[O:2])=[CH:9][CH:10]=[C:11]([CH3:12])[C:6]=1[Br:5]

참가 물질

4

반응물 2

HCID 944Nitric AcidHCID 684712-Bromo-m-xylene

생성물 1

HCID 123959052-Bromo-1,3-dimethyl-4-nitrobenzene

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

Fuming nitric acid (>90% yellow fuming HNO3) is slowly added to a solution of 2-bromo-m-xylene (20 g, 150 mmol) in acetic acid (100 ml) cooled in an ice bath (above freezing point). The resulting mixture is allowed to warm to room temperature, stirred for 1 hour, and heated at 80° C. for 2 hours or until the reaction is shown to be complete by GC/MS analysis following micro-scale base work-up. The reaction mixture is cooled to room temperature and poured into ice/water with stirring. The resulting yellow precipitates are collected by suction filtration and air dried to obtain 2,6-dimethyl-3-nitrobromobenzene.

후처리

  1. temperaturecooled in an ice bath (above freezing point)
  2. temperatureheated at 80° C. for 2 hours or until the reaction
  3. temperatureThe reaction mixture is cooled to room temperature
  4. stirringwith stirring
  5. customThe resulting yellow precipitates
  6. filtrationare collected by suction filtration and air
  7. customdried

출처 및 근거

ORD 기록
ord-be524cb8b1a6445599b71a2c69566762
출처 데이터셋
uspto-grants-2005_02
특허 번호
US06858637B2

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