Phenylphosphonic dichloride → 2-Chloro-3,4-diethoxycarbonyl-6-methyl-5-nitropyridine

HRID 37476

反応式

HRID 37476 の反応式
[CH2:1]([O:3][C:4]([C:6]1[C:7](=O)[NH:8][C:9]([CH3:20])=[C:10]([N+:17]([O-:19])=[O:18])[C:11]=1[C:12]([O:14][CH2:15][CH3:16])=[O:13])=[O:5])[CH3:2].C1(P(Cl)([Cl:30])=O)C=CC=CC=1>O>[Cl:30][C:7]1[C:6]([C:4]([O:3][CH2:1][CH3:2])=[O:5])=[C:11]([C:12]([O:14][CH2:15][CH3:16])=[O:13])[C:10]([N+:17]([O-:19])=[O:18])=[C:9]([CH3:20])[N:8]=1

参加物

4

反応物 2

HCID 69990Phenylphosphonic dichlorideHCID 199355903,4-Diethoxycarbonyl-6-methyl-5-nitro-2-pyridone

生成物 1

HCID 199355842-Chloro-3,4-diethoxycarbonyl-6-methyl-5-nitropyridine

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
170 °C

実験手順

To 1.0 g of 3,4-diethoxycarbonyl-6-methyl-5-nitro-2-pyridone was added 1.3 ml (3.2 eq.) of phenylphosphonic dichloride. The mixture was heated at 170° C. for 20 mintues. Water was added to the reaction mixture, followed by extraction with ethyl acetate. The organic layer was washed with water and a saturated aqueous solution of sodium chloride and dried over magnesium sulfate. After the solvent was distilled off, the residue was purified by silica gel column chromatography (eluent:ethyl acetate) to give an oily product.

後処理

  1. extractionfollowed by extraction with ethyl acetate
  2. washThe organic layer was washed with water
  3. dry with materiala saturated aqueous solution of sodium chloride and dried over magnesium sulfate
  4. distillationAfter the solvent was distilled off
  5. customthe residue was purified by silica gel column chromatography (eluent:ethyl acetate)
  6. customto give an oily product

出典と根拠

ORDレコード
ord-1ee93671a1c449ee91ceaa24da712e78
出典データセット
uspto-grants-1995_05
特許番号
US05420275

関連ノート

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