4-Chloro-1,2-dinitrobenzene → ethyl P-methyl-2-nitro-5-chlorophenylphosphinate

HRID 463560

反応式

HRID 463560 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([N+:8]([O-:10])=[O:9])=[C:4]([N+]([O-])=O)[CH:3]=1.[CH3:14][P:15]([O:19]CC)[O:16][CH2:17][CH3:18]>C(#N)C>[CH3:14][P:15]([C:4]1[CH:3]=[C:2]([Cl:1])[CH:7]=[CH:6][C:5]=1[N+:8]([O-:10])=[O:9])(=[O:19])[O:16][CH2:17][CH3:18]

参加物

4

反応物 2

HCID 330974-Chloro-1,2-dinitrobenzeneHCID 85063Diethyl methylphosphonite

生成物 1

HCID 53860251ethyl P-methyl-2-nitro-5-chlorophenylphosphinate

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

To 4-chloro-1,2-dinitrobenzene (13.2 g, 65.0 mmol) dissolved in acetonitrile (150 ml) is added, dropwise, diethyl methylphosphonite (16.0 g, 117.6 mmol). The mixture is stirred at RT for 20 hours, after which it is concentrated. The crude product is purified by column chromatography (developing with 50% ethyl acetate/hexane) to yield ethyl P-methyl-2-nitro-5-chlorophenylphosphinate.

後処理

  1. additionis added
  2. concentrationafter which it is concentrated
  3. customThe crude product is purified by column chromatography (developing with 50% ethyl acetate/hexane)

出典と根拠

ORDレコード
ord-cd5e6dca7b5048fab9a1583e2647bcfa
出典データセット
uspto-grants-1985_05
特許番号
US04520197

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