Ethyl Acetate → 1,5-Dimethoxy-2,4-dinitrobenzene

HRID 1285267ノート

反応式

HRID 1285267 の反応式
Cl[C:2]1[CH:7]=[C:6](Cl)[C:5]([N+:9]([O-:11])=[O:10])=[CH:4][C:3]=1[N+:12]([O-:14])=[O:13].[CH3:15][O-:16].[Na+].[C:18](OCC)(=[O:20])C>CO>[CH3:18][O:20][C:2]1[CH:7]=[C:6]([O:16][CH3:15])[C:5]([N+:9]([O-:11])=[O:10])=[CH:4][C:3]=1[N+:12]([O-:14])=[O:13]

参加物

5

反応物 3

HCID 8857Ethyl AcetateHCID 772861,3-Dichloro-4,6-dinitrobenzeneHCID 10942334Sodium Methoxide

生成物 1

HCID 6150531,5-Dimethoxy-2,4-dinitrobenzene

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

To 20.0 g (0.084 moles) 1,5-dichloro-2,4-dinitrobenzene in 200 ml methanol is added 22.7 g (0.42 moles) sodium methoxide. The mixture is heated to reflux and the reaction is monitored by TLC (ethyl acetate). TLC after approximately 12 hours shows the reaction is complete. The host mixture is poured into 750 ml ice/H2O. The pale yellow precipitate is collected by vacuum filtration and dried in the vacuum oven at 50° C. Yield is 16.3 g (85.7%). Recrystallization using toluene and 1 g decolorizing charcoal yields 11.5 g product, m.p. 153°-155° C.

後処理

  1. temperatureThe mixture is heated
  2. temperatureto reflux
  3. filtrationThe pale yellow precipitate is collected by vacuum filtration
  4. customdried in the vacuum oven at 50° C
  5. customRecrystallization

出典と根拠

ORDレコード
ord-98ac8f8646be4fc397764259d288cfbc
出典データセット
uspto-grants-1986_01
特許番号
US04566876

反応ノート

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