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

HRID 1285267

반응식

HRID 1285267 반응식
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]

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-98ac8f8646be4fc397764259d288cfbc
출처 데이터셋
uspto-grants-1986_01
특허 번호
US04566876

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