Pyridine → HCID 19935586, 화합물

HRID 37500

반응식

HRID 37500 반응식
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]

참가 물질

5

반응물 3

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

생성물 1

HCID 19935586HCID 19935586, 화합물

시약·촉매·용매 1

HCID 111,2-Dichloroethane용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-fe046a86aab84ef0b6811df7ef1c1e4c
출처 데이터셋
uspto-grants-1995_05
특허 번호
US05420275

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