Ammonium Chloride → HCID 66613369、化合物

HRID 406574ノート

反応式

HRID 406574 の反応式
[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]

参加物

6

反応物 2

HCID 25517Ammonium ChlorideHCID 666141515-(2-chloro-4-fluorophenyl)-1,3-dimethyl-4-nitro-1H-pyrazole2 回

生成物 1

HCID 66613369HCID 66613369、化合物

試薬・触媒・溶媒 3

HCID 23925Iron触媒HCID 702Ethanol溶媒HCID 8857Ethyl Acetate溶媒

反応条件

温度
80 °C

実験手順

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).

後処理

  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)

出典と根拠

ORDレコード
ord-72847333c3c34584999175d34cdd44cc
出典データセット
uspto-grants-2014_06
特許番号
US08754115B2

反応ノート

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