Ammonium Chloride → HCID 66839376, 화합물

HRID 546736노트

반응식

HRID 546736 반응식
[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]

참가 물질

6

반응물 2

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

생성물 1

HCID 66839376HCID 66839376, 화합물수율 100%

시약·촉매·용매 3

HCID 23925Iron촉매HCID 702Ethanol용매HCID 962Water용매

반응 조건

온도
100 °C

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-9adabb96afb84bb5b73551b05f704639
출처 데이터셋
uspto-grants-2011_05
특허 번호
US07935815B2

반응 노트

불러오는 중…