Ammonium Chloride → HCID 66613369, 화합물

HRID 2276004노트

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HRID 2276004 반응식
[Cl:1][C:2]1[CH:7]=[C:6]([F:8])[CH:5]=[CH:4][C:3]=1[C:9]1[N:13]([CH3:14])[N:12]=[C:11]([CH3:15])[C:10]=1[N+:16]([O-])=O.[Cl-].[NH4+]>C(O)C.C(OCC)(=O)C.[Fe]>[Cl:1][C:2]1[CH:7]=[C:6]([F:8])[CH:5]=[CH:4][C:3]=1[C:9]1[N:13]([CH3:14])[N:12]=[C:11]([CH3:15])[C:10]=1[NH2:16]

참가 물질

6

반응물 2

HCID 25517Ammonium ChlorideHCID 666141515-(2-chloro-4-fluorophenyl)-1,3-dimethyl-4-nitro-1H-pyrazole2회

생성물 1

HCID 66613369HCID 66613369, 화합물

시약·촉매·용매 3

HCID 23925Iron촉매HCID 702Ethanol용매HCID 8857Ethyl Acetate용매

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온도
80 °C

실험 절차

A mixture of 5-(2-chloro-4-fluorophenyl)-1,3-dimethyl-4-nitro-1H-pyrazole (i.e. the product of Step A) (0.2 g, 0.74 mmol), iron powder (0.2 g, 3.6 mmol) and saturated aqueous ammonium chloride solution (1 mL) in ethanol (5 mL) was heated at 80° C. for 4 h. After cooling to room temperature, the reaction mixture was diluted with ethyl acetate and filtered through a pad of Celite® (diatomaceous earth) on a sintered glass frit funnel. The filtrate was concentrated under reduced pressure and the resulting material was purified by silica gel column chromatography (ethyl acetate as eluant) to provide the title compound (0.14 g).

후처리

  1. temperatureAfter cooling to room temperature
  2. filtrationfiltered through a pad of Celite® (diatomaceous earth) on a sintered glass frit funnel
  3. concentrationThe filtrate was concentrated under reduced pressure
  4. customthe resulting material was purified by silica gel column chromatography (ethyl acetate as eluant)

출처 및 근거

ORD 기록
ord-635ba35e5dfd477badc2b076a64eff08
출처 데이터셋
uspto-grants-2015_09
특허 번호
US09131693B2

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