Ethanol → 3,4-Dichlorobenzene-1,2-diamine

HRID 1167090

반응식

HRID 1167090 반응식
[Cl:1][C:2]1[C:8]([Cl:9])=[CH:7][CH:6]=[C:5]([N+:10]([O-])=O)[C:3]=1[NH2:4].C(O)C.[H][H]>O.[Ni]>[Cl:1][C:2]1[C:3]([NH2:4])=[C:5]([NH2:10])[CH:6]=[CH:7][C:8]=1[Cl:9]

참가 물질

6

반응물 3

HCID 702EthanolHCID 30175542,3-Dichloro-6-nitroanilineHCID 178418361HCID 178418361, 화합물

생성물 1

HCID 108450203,4-Dichlorobenzene-1,2-diamine수율 95%

시약·촉매·용매 2

HCID 935Nickel촉매HCID 962Water용매

실험 절차

2,3-Dichloro-6-nitroaniline (20.11 g, 97.14 mmol), Raney-nickel (4.78 g of a 50% slurry in water), and ethanol (250 mL) were combined in an autoclave which was presssurized to 150 psig with hydrogen The resulting reaction mixture was allowed to stir at RT overnight. The mixture was then filtered through a pad of celite, which was subsequently washed with several portions of methanol, and the solvents were removed by rotary evaporation to leave a dark brown solid. The solid was slurried and in hexanes and was collected on a Büchner funnel to afford 16.31 g (95%) of a brown solid. MS (EI): m/z 177.0 (M+H).

후처리

  1. customThe resulting reaction mixture
  2. filtrationThe mixture was then filtered through a pad of celite, which
  3. washwas subsequently washed with several portions of methanol
  4. customthe solvents were removed by rotary evaporation
  5. customto leave a dark brown solid
  6. customwas collected on a Büchner funnel

출처 및 근거

ORD 기록
ord-5ee293604ae44286a3bd1eb12a31fb30
출처 데이터셋
uspto-grants-2003_09
특허 번호
US06617315B1

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