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

HRID 545072노트

반응식

HRID 545072 반응식
[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]

참가 물질

6

반응물 2

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

생성물 1

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

시약·촉매·용매 3

HCID 23925Iron촉매HCID 702Ethanol용매HCID 962Water용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-c228b34c3a074790ad74b0874218dd10
출처 데이터셋
uspto-grants-2011_05
특허 번호
US07935702B2

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