4-Nitrobenzaldehyde → Diethyl [2-(4-nitrophenyl)ethenyl]phosphonate

HRID 1378966노트

반응식

HRID 1378966 반응식
CC[O-].[Na+].[N+:5]([C:8]1[CH:15]=[CH:14][C:11]([CH:12]=O)=[CH:10][CH:9]=1)([O-:7])=[O:6].[CH2:16](P(=O)(OCC)OCC)[P:17](=[O:24])([O:21][CH2:22][CH3:23])[O:18][CH2:19][CH3:20]>CO>[CH2:19]([O:18][P:17]([CH:16]=[CH:12][C:11]1[CH:14]=[CH:15][C:8]([N+:5]([O-:7])=[O:6])=[CH:9][CH:10]=1)(=[O:24])[O:21][CH2:22][CH3:23])[CH3:20]

참가 물질

5

반응물 3

HCID 5414-NitrobenzaldehydeHCID 15455Tetraethyl methylenediphosphonateHCID 2723922Sodium ethoxide2회

생성물 1

HCID 53749636Diethyl [2-(4-nitrophenyl)ethenyl]phosphonate

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

Sodium ethylate (4.95 g, 72.8 mmol) is added to a solution of 4-nitrobenzaldehyde (10 g, 66.2 mmol) in 200 ml of methanol, and tetraethyl methylenediphosphonate (21 g, 72.8 mmol) is then added dropwise. After 2 h of stirring at room temperature, a further 0.43 g of sodium ethylate and 2 g of tetraethyl methylene diphosphonate are added. After 15 min of stirring at room temperature, the ethanol is evaporated off under vacuum and the residue is bipartitioned in a water/ethyl acetate mixture. The organic phase is washed with water, then dried (MgSO4) and evaporated under vacuum to give the expected product.

후처리

  1. additionis then added dropwise
  2. stirringAfter 15 min of stirring at room temperature
  3. customthe ethanol is evaporated off under vacuum
  4. washThe organic phase is washed with water
  5. dry with materialdried (MgSO4)
  6. customevaporated under vacuum

출처 및 근거

ORD 기록
ord-ccec20dabff04adea36862d19b735e8c
출처 데이터셋
uspto-grants-1997_09
특허 번호
US05670493

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