Acetic Acid → Hydrochloric Acid

HRID 1890483노트

반응식

HRID 1890483 반응식
[Cl:1][C:2]1[C:7]([Cl:8])=[CH:6][C:5](CN)=[C:4]([N+:11]([O-])=O)[CH:3]=1.O.[NH3:15].[ClH:16].[C:17](O)(=O)C>CCOCC.[Zn].C(OCC)(=O)C>[Cl:16][C:6]1[CH:5]=[C:4]([NH2:11])[C:3]([NH:15][CH3:17])=[CH:2][C:7]=1[Cl:8].[ClH:1]

참가 물질

10

반응물 5

HCID 176Acetic AcidHCID 222AmmoniaHCID 313Hydrochloric AcidHCID 962WaterHCID 86762003HCID 86762003, 화합물

생성물 2

HCID 313Hydrochloric AcidHCID 30163614,5-Dichloro-2-(methylamino)aniline

시약·촉매·용매 3

HCID 23994Zinc촉매HCID 3283Diethyl Ether용매HCID 8857Ethyl Acetate용매

반응 조건

온도
20 °C

실험 절차

A solution of (4,5-dichloro-2-nitrophenyl)methylamine (500 mg) in acetic acid (7.5 ml) is treated portionwise with zinc powder (740 mg). The reaction medium is stirred at ambient temperature (20° C.) until complete reduction. Water (13 ml) and 28% ammonia are added to pH 7, and then the reaction medium is depleted using ethyl acetate (3×50). The organic extracts are combined, dried over magnesium sulphate, filtered and evaporated under reduced pressure. The oil obtained is taken up in ether (50 ml) and then 2N HCl is added thereto. The solid formed is filtered off. 4,5-Dichloro-N-methylbenzene-1,2-diamine is isolated in its hydrochloride form (510 mg), and is used in the next state.

후처리

  1. dry with materialdried over magnesium sulphate
  2. filtrationfiltered
  3. customevaporated under reduced pressure
  4. customThe oil obtained
  5. customThe solid formed
  6. filtrationis filtered off

출처 및 근거

ORD 기록
ord-2cd6ad61e32741778dbab9ee17783480
출처 데이터셋
uspto-grants-2013_08
특허 번호
US08507483B2

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