2-Chloro-5-nitro-3-(trifluoromethyl)pyridine → 6-Chloro-5-(trifluoromethyl)pyridin-3-amine

HRID 545072ノート

反応式

HRID 545072 の反応式
[Cl:1][C:2]1[C:7]([C:8]([F:11])([F:10])[F:9])=[CH:6][C:5]([N+:12]([O-])=O)=[CH:4][N:3]=1.[Cl-].[Ca+2].[Cl-]>C(O)C.O.[Fe]>[Cl:1][C:2]1[N:3]=[CH:4][C:5]([NH2:12])=[CH:6][C:7]=1[C:8]([F:11])([F:9])[F:10]

参加物

6

反応物 2

HCID 38491402-Chloro-5-nitro-3-(trifluoromethyl)pyridineHCID 5284359Calcium Chloride

生成物 1

HCID 135322446-Chloro-5-(trifluoromethyl)pyridin-3-amine

試薬・触媒・溶媒 3

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

実験手順

Heat a mixture of 2-chloro-5-nitro-3-trifluoromethyl-pyridine (2.27 g, 10 mmol), calcium chloride (1.1 g, 10 mmol) and iron powder (4.5 g) in ethanol (30 mL) and water (5 mL) at reflux for 1 hour. Cool the mixture and filter through Celite. Evaporate the filtrate, dissolve the residue in EtOAc (200 mL) and wash with saturated NaHCO3(aq) (100 mL) and brine (100 mL). Dry the organic extract over MgSO4 and remove the solvent under reduced pressure to yield the title compound.

後処理

  1. temperatureHeat
  2. temperatureat reflux for 1 hour
  3. temperatureCool the mixture
  4. filtrationfilter through Celite
  5. customEvaporate the filtrate
  6. dissolutiondissolve the residue in EtOAc (200 mL)
  7. washwash with saturated NaHCO3(aq) (100 mL) and brine (100 mL)
  8. customDry the
  9. extractionorganic extract over MgSO4
  10. customremove the solvent under reduced pressure

出典と根拠

ORDレコード
ord-c228b34c3a074790ad74b0874218dd10
出典データセット
uspto-grants-2011_05
特許番号
US07935702B2

反応ノート

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