Pyridine → HCID 19935586、化合物

HRID 37500

反応式

HRID 37500 の反応式
Cl[C:2]1[C:7]([C:8]([O:10][CH2:11][CH3:12])=[O:9])=[C:6]([C:13]([O:15][CH2:16][CH3:17])=[O:14])[C:5]([N+:18]([O-:20])=[O:19])=[C:4]([C:21]2[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=2)[N:3]=1.[NH:27]1[CH:31]=[N:30][CH:29]=[N:28]1.N1C=CC=CC=1>ClCCCl>[CH2:11]([O:10][C:8]([C:7]1[C:2]([N:27]2[CH:31]=[N:30][CH:29]=[N:28]2)=[N:3][C:4]([C:21]2[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=2)=[C:5]([N+:18]([O-:20])=[O:19])[C:6]=1[C:13]([O:15][CH2:16][CH3:17])=[O:14])=[O:9])[CH3:12]

参加物

5

反応物 3

HCID 1049PyridineHCID 92571H-1,2,4-TriazoleHCID 199355872-Chloro-3,4-diethoxycarbonyl-5-nitro-6-phenylpyridine

生成物 1

HCID 19935586HCID 19935586、化合物

試薬・触媒・溶媒 1

HCID 111,2-Dichloroethane溶媒

実験手順

A mixture of 0.379 g of 2-chloro-3,4-diethoxycarbonyl-5-nitro-6-phenylpyridine, 0.2 g of (1H-1,2,4-triazole, 0.2 ml of pyridine and 15 ml of 1,2-dichloroethane was reacted at 80° C. for 18 hours. After the reaction mixture was concentrated, the concentrate was extracted with ethyl acetate. The extract was washed with water and a saturated aqueous solution of sodium chloride and dried over sodium sulfate. After the solvent was distilled off, the residue was subjected to silica gel column chromatography (eluent:dichloromethane/ethyl acetate 4:1), to give 0.19 g of the title compound as yellow crystals.

後処理

  1. customwas reacted at 80° C. for 18 hours
  2. concentrationAfter the reaction mixture was concentrated
  3. extractionthe concentrate was extracted with ethyl acetate
  4. washThe extract was washed with water
  5. dry with materiala saturated aqueous solution of sodium chloride and dried over sodium sulfate
  6. distillationAfter the solvent was distilled off

出典と根拠

ORDレコード
ord-fe046a86aab84ef0b6811df7ef1c1e4c
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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