Nitric Acid → 1,4-Dimethoxy-2-methyl-5-nitrobenzene

HRID 2114354

반응식

HRID 2114354 반응식
[CH3:1][C:2]1[CH:7]=[C:6]([O:8][CH3:9])[CH:5]=[CH:4][C:3]=1[O:10][CH3:11].[N+:12]([O-])([OH:14])=[O:13]>C(O)(=O)C>[CH3:1][C:2]1[CH:7]=[C:6]([O:8][CH3:9])[C:5]([N+:12]([O-:14])=[O:13])=[CH:4][C:3]=1[O:10][CH3:11]

참가 물질

4

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온도
40 °C

실험 절차

2-Methyl-1,4-bis(methyloxy)benzene (6.12 g, 40 mmol) was dissolved in acetic acid (20 mL) and heated at 40° C. A solution of nitric acid (4.32 g) in acetic acid (10 mL) was added to above solution drop wise over 5 minutes. The reaction mixture was stirred at 40° C. for 30 min (yellow precipitates formed), then room temperature for 30 min and then diluted with water (300 mL). The precipitate was collected by filtration, washed with water, and dried in the air for 16 h to afford the title compound (7.56 g, 96%) as a yellow solid. MS (ES) m/e 198 [M+H]+.

후처리

  1. custom(yellow precipitates formed)
  2. waitroom temperature for 30 min
  3. additiondiluted with water (300 mL)
  4. filtrationThe precipitate was collected by filtration
  5. washwashed with water
  6. customdried in the air for 16 h

출처 및 근거

ORD 기록
ord-e0f63a35e0e4449c8d059001b5d17342
출처 데이터셋
uspto-grants-2008_10
특허 번호
US07432258B2

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