Acetic Acid → HCID 19834631、化合物

HRID 2051065ノート

反応式

HRID 2051065 の反応式
[H][H].O.C(O)(=O)C.[N+:8]([C:11]1[C:12]([O:24][CH2:25][CH3:26])=[C:13]([Cl:23])[CH:14]=[C:15]([N+:20]([O-])=O)[C:16]=1[O:17][CH2:18][CH3:19])([O-])=O>[Fe].C(OCC)(=O)C>[ClH:23].[CH2:25]([O:24][C:12]1[C:11]([NH2:8])=[C:16]([O:17][CH2:18][CH3:19])[C:15]([NH2:20])=[CH:14][C:13]=1[Cl:23])[CH3:26]

参加物

7

反応物 4

HCID 176Acetic AcidHCID 962WaterHCID 19751981HCID 19751981、化合物HCID 178418361HCID 178418361、化合物

生成物 1

HCID 19834631HCID 19834631、化合物

試薬・触媒・溶媒 2

HCID 23925Iron触媒2 回HCID 8857Ethyl Acetate溶媒

反応条件

温度
80 °C

実験手順

170 g of powdered iron which had been reduced with hydrogen were added to 450 ml of water containing 8.5 ml of acetic acid which have previously been heated to 80° C., and then 0.3 mole (87 g) of 3,5-dinitro-2,4-diethoxychlorobenzene was then gradually added with stirring. Upon completion of the additions, the reaction mixture was maintained in a boiling water bath for 30 additional minutes. After cooling, the reaction mixture was centrifuged. The iron slurries were made to a paste again with ethyl acetate and the mother liquors were extracted with ethyl acetate. The ethyl acetate phases, joined together, were washed with water and then dried over Na2SO4. Upon addition of a hydrochloric acid solution in ethanol, the expected product precipitated. After thorough draining, it was washed with acetone. It was recrystallized from an aqueous-alcoholic solution of hydrochloric acid.

後処理

  1. temperatureUpon completion of the additions, the reaction mixture was maintained in a boiling water bath for 30 additional minutes
  2. temperatureAfter cooling
  3. extractionthe mother liquors were extracted with ethyl acetate
  4. washwere washed with water
  5. dry with materialdried over Na2SO4
  6. additionUpon addition of a hydrochloric acid solution in ethanol
  7. customthe expected product precipitated
  8. washAfter thorough draining, it was washed with acetone
  9. customIt was recrystallized from an aqueous-alcoholic solution of hydrochloric acid

出典と根拠

ORDレコード
ord-30f90d2f6a594ebaba6159219d607982
出典データセット
uspto-grants-1991_05
特許番号
US05015772

反応ノート

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