Ammonium Chloride → HCID 66839376、化合物

HRID 546736ノート

反応式

HRID 546736 の反応式
[Cl-].[NH4+].[CH3:3][O:4][C:5]1[N:10]=[C:9](/[CH:11]=[CH:12]/[C:13]([O:15][CH2:16][CH3:17])=[O:14])[CH:8]=[CH:7][C:6]=1[N+:18]([O-])=O>C(O)C.O.[Fe]>[NH2:18][C:6]1[CH:7]=[CH:8][C:9](/[CH:11]=[CH:12]/[C:13]([O:15][CH2:16][CH3:17])=[O:14])=[N:10][C:5]=1[O:4][CH3:3]

参加物

6

反応物 2

HCID 25517Ammonium ChlorideHCID 66839168ethyl (E)-3-(6-methoxy-5-nitropyridin-2-yl)acrylate

生成物 1

HCID 66839376HCID 66839376、化合物収率 100%

試薬・触媒・溶媒 3

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

反応条件

温度
100 °C

実験手順

Iron (3.72 g) and ammonium chloride (7.13 g) were added to a solution of ethyl (E)-3-(6-methoxy-5-nitropyridin-2-yl)acrylate (2.1 g) in ethanol (100 mL) and water (20 mL). The reaction solution was stirred at 100° C. for one hour and then left to cool to room temperature. The reaction solution was filtered through celite. Ethyl acetate was added and the organic layer was separated. The resulting organic layer was washed with saturated sodium bicarbonate water and brine, dried over anhydrous magnesium sulfate and then concentrated under reduced pressure. The residue was purified by silica gel column chromatography (elution solvent: heptane-ethyl acetate system) to obtain 1.85 g of the title compound. The property values of the compound are as follows.

後処理

  1. waitleft
  2. temperatureto cool to room temperature
  3. filtrationThe reaction solution was filtered through celite
  4. additionEthyl acetate was added
  5. customthe organic layer was separated
  6. washThe resulting organic layer was washed with saturated sodium bicarbonate water and brine
  7. dry with materialdried over anhydrous magnesium sulfate
  8. concentrationconcentrated under reduced pressure
  9. customThe residue was purified by silica gel column chromatography (elution solvent: heptane-ethyl acetate system)

出典と根拠

ORDレコード
ord-9adabb96afb84bb5b73551b05f704639
出典データセット
uspto-grants-2011_05
特許番号
US07935815B2

反応ノート

読み込み中…