Ethanol → Ethyl 2,5-dichloronicotinate

HRID 493569

반응식

HRID 493569 반응식
[Cl:1][C:2]1[N:10]=[CH:9][C:8]([Cl:11])=[CH:7][C:3]=1[C:4]([OH:6])=[O:5].[CH2:12](O)[CH3:13].S(=O)(=O)(O)O.C(=O)(O)[O-].[Na+]>C1(C)C=CC=CC=1>[Cl:1][C:2]1[N:10]=[CH:9][C:8]([Cl:11])=[CH:7][C:3]=1[C:4]([O:6][CH2:12][CH3:13])=[O:5]

참가 물질

6

반응물 4

HCID 702EthanolHCID 1118Sulfuric AcidHCID 516892Sodium BicarbonateHCID 27360852,5-Dichloropyridine-3-carboxylic acid

생성물 1

HCID 5200405Ethyl 2,5-dichloronicotinate

시약·촉매·용매 1

HCID 1140Toluene용매

반응 조건

온도
130 °C

실험 절차

To a solution of 2,5-dichloronicotinic acid (30 g, 0.16 mol) in toluene (100 ml) was added ethanol (50 ml) and conc. sulfuric acid (1 ml). The reaction mixture was heated at 130° C. for 3 days with stirring. Then the reaction mixture was cooled and poured into sat. sodium bicarbonate solution. The whole mixture was extracted with ethyl acetate. The organic phase was washed with brine, dried (sodium sulfate), and concentrated to afford 34 g (quant.) of title compound:

후처리

  1. temperatureThen the reaction mixture was cooled
  2. extractionThe whole mixture was extracted with ethyl acetate
  3. washThe organic phase was washed with brine
  4. dry with materialdried (sodium sulfate)
  5. concentrationconcentrated

출처 및 근거

ORD 기록
ord-3991b91846c94e3bb9581a3fdd1b60eb
출처 데이터셋
uspto-grants-2009_05
특허 번호
US07534914B2

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