Ammonium Chloride → HCID 54401849、化合物

HRID 1378967ノート

反応式

HRID 1378967 の反応式
[CH2:1]([O:3][P:4]([CH:9]=[CH:10][C:11]1[CH:16]=[CH:15][C:14]([N+:17]([O-])=O)=[CH:13][CH:12]=1)(=[O:8])[O:5][CH2:6][CH3:7])[CH3:2].[Cl-].[NH4+]>[Fe]>[CH2:6]([O:5][P:4]([CH:9]=[CH:10][C:11]1[CH:16]=[CH:15][C:14]([NH2:17])=[CH:13][CH:12]=1)(=[O:8])[O:3][CH2:1][CH3:2])[CH3:7]

参加物

4

反応物 2

HCID 25517Ammonium ChlorideHCID 53749636Diethyl [2-(4-nitrophenyl)ethenyl]phosphonate

生成物 1

HCID 54401849HCID 54401849、化合物

試薬・触媒・溶媒 1

HCID 23925Iron触媒

実験手順

A suspension containing 4-nitrostyrylphosphonic acid diethyl ester (3.0 g, 10.5 mmol), iron powder (5.58 g, 100 mmol) and ammonium chloride (5.58 g, 104 mmol) is heated to reflux for 45 minutes. The reaction medium is filtered through Celite. The filtrate is concentrated under vacuum and is bipartitioned in a water/dichloromethane mixture. The organic phase is washed with water, then dried (MgSO4) and evaporated under vacuum to give the expected product, which crystallizes gradually.

後処理

  1. temperatureis heated
  2. temperatureto reflux for 45 minutes
  3. filtrationThe reaction medium is filtered through Celite
  4. concentrationThe filtrate is concentrated under vacuum
  5. washThe organic phase is washed with water
  6. dry with materialdried (MgSO4)
  7. customevaporated under vacuum

出典と根拠

ORDレコード
ord-1d84d78604e14006bc7cc888c2d45c30
出典データセット
uspto-grants-1997_09
特許番号
US05670493

反応ノート

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