Acetic Acid → Hydrochloric Acid

HRID 1890483ノート

反応式

HRID 1890483 の反応式
[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]

参加物

10

反応物 5

HCID 176Acetic AcidHCID 222AmmoniaHCID 313Hydrochloric AcidHCID 962WaterHCID 86762003HCID 86762003、化合物

生成物 2

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

試薬・触媒・溶媒 3

HCID 23994Zinc触媒HCID 3283Diethyl Ether溶媒HCID 8857Ethyl Acetate溶媒

反応条件

温度
20 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-2cd6ad61e32741778dbab9ee17783480
出典データセット
uspto-grants-2013_08
特許番号
US08507483B2

反応ノート

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