Ammonium Chloride → 4-Benzyloxy-3-chloroaniline

HRID 1013914ノート

反応式

HRID 1013914 の反応式
[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

参加物

6

反応物 2

HCID 25517Ammonium ChlorideHCID 3085094-Benzyloxy-3-chloronitrobenzene

生成物 1

HCID 12682854-Benzyloxy-3-chloroaniline収率 95.9%

試薬・触媒・溶媒 3

HCID 23925Iron触媒HCID 702Ethanol溶媒HCID 962Water溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-78882305ae6a446baa474dc23978d36c
出典データセット
uspto-grants-2011_07
特許番号
US07982043B2

反応ノート

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