Acetic Acid → HCID 19751973, 화합물

HRID 1607485노트

반응식

HRID 1607485 반응식
[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].[ClH:23].[NH2:8][C:11]1[C:12]([O:24][CH2:25][CH3:26])=[C:13]([Cl:23])[CH:14]=[C:15]([NH2:20])[C:16]=1[O:17][CH2:18][CH3:19]

참가 물질

7

반응물 4

HCID 176Acetic AcidHCID 962WaterHCID 19751981HCID 19751981, 화합물HCID 178418361HCID 178418361, 화합물

생성물 1

HCID 19751973HCID 19751973, 화합물

시약·촉매·용매 2

HCID 23925Iron촉매2회HCID 8857Ethyl Acetate용매

반응 조건

온도
80 °C

실험 절차

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 had previously been heated to 80° C., and then 0.3 mole (87 g) of 3,5-dinitro-2,4-diethoxychlorobenzene was added gradually, 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.

후처리

  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. washThe ethyl acetate phases joined together were 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

출처 및 근거

ORD 기록
ord-a9544eada1094080ad8d949edc553a0b
출처 데이터셋
uspto-grants-1989_09
특허 번호
US04865618

반응 노트

불러오는 중…