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

HRID 2354350ノート

反応式

HRID 2354350 の反応式
[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]

参加物

4

反応物 2

HCID 944Nitric AcidHCID 905522,5-Dimethoxytoluene

生成物 1

HCID 27780951,4-Dimethoxy-2-methyl-5-nitrobenzene収率 96%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒2 回

反応条件

温度
40 °C

実験手順

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]+.

後処理

  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

出典と根拠

ORDレコード
ord-6f213d45c25d4af2beb3c168f271ce53
出典データセット
uspto-grants-2010_07
特許番号
US07749998B2

反応ノート

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