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

HRID 37476

반응식

HRID 37476 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
170 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-1ee93671a1c449ee91ceaa24da712e78
출처 데이터셋
uspto-grants-1995_05
특허 번호
US05420275

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