Ammonium Chloride → 4-Benzyloxy-3-chloroaniline

HRID 1013914

반응식

HRID 1013914 반응식
[CH2:1]([O:8][C:9]1[CH:14]=[CH:13][C:12]([N+:15]([O-])=O)=[CH:11][C:10]=1[Cl:18])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[Cl-].[NH4+]>C(O)C.O.[Fe]>[CH2:1]([O:8][C:9]1[CH:14]=[CH:13][C:12]([NH2:15])=[CH:11][C:10]=1[Cl:18])[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

참가 물질

6

반응물 2

HCID 25517Ammonium ChlorideHCID 3085094-Benzyloxy-3-chloronitrobenzene

생성물 1

HCID 12682854-Benzyloxy-3-chloroaniline수율 95.9%

시약·촉매·용매 3

HCID 23925Iron촉매HCID 702Ethanol용매HCID 962Water용매

실험 절차

A mixture of 6.59 g (0.025 moles) of the 4-benzyloxy-3-chloro nitrobenzene (example 4), 4.19 g (0.075 moles) of iron powder, and 12.04 g (0.225 moles) of ammonium chloride in 100 ml of ethanol and 25 ml of water was stirred mechanically and refluxed for half an hour. The reaction was allowed to cool and stir for 1 hour. The mixture was filtered and solids were washed with ethanol. The combined filtrates were taken to dryness in vacuo. This solid was dissolved in methylene chloride and passed through Magnesol. Removal of the solvent from the filtrate in vacuo gave 5.60 g of title compound.

후처리

  1. temperaturerefluxed for half an hour
  2. temperatureto cool
  3. stirringstir for 1 hour
  4. filtrationThe mixture was filtered
  5. washsolids were washed with ethanol
  6. dissolutionThis solid was dissolved in methylene chloride
  7. customRemoval of the solvent from the filtrate in vacuo

출처 및 근거

ORD 기록
ord-78882305ae6a446baa474dc23978d36c
출처 데이터셋
uspto-grants-2011_07
특허 번호
US07982043B2

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