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

HRID 2354350

반응식

HRID 2354350 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

반응물 2

HCID 944Nitric AcidHCID 905522,5-Dimethoxytoluene

생성물 1

HCID 27780951,4-Dimethoxy-2-methyl-5-nitrobenzene수율 96%

시약·촉매·용매 1

HCID 176Acetic Acid용매2회

반응 조건

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-6f213d45c25d4af2beb3c168f271ce53
출처 데이터셋
uspto-grants-2010_07
특허 번호
US07749998B2

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