Dimethylformamide → ethyl 4,6-dichloro-3-formyl-1H-indole-2-carboxylate

HRID 568185

반응식

HRID 568185 반응식
[C:1]([C:6]1[NH:7][C:8]2[C:13]([CH:14]=1)=[C:12]([Cl:15])[CH:11]=[C:10]([Cl:16])[CH:9]=2)([O:3][CH2:4][CH3:5])=[O:2].CN(C)[CH:19]=[O:20].P(Cl)(Cl)(Cl)=O>ClC(Cl)C>[CH:19]([C:14]1[C:13]2[C:8](=[CH:9][C:10]([Cl:16])=[CH:11][C:12]=2[Cl:15])[NH:7][C:6]=1[C:1]([O:3][CH2:4][CH3:5])=[O:2])=[O:20]

참가 물질

5

반응물 3

HCID 6228DimethylformamideHCID 24813Phosphorus oxychlorideHCID 2736407ethyl 4,6-dichloro-1H-indole-2-carboxylate

생성물 1

HCID 2794948ethyl 4,6-dichloro-3-formyl-1H-indole-2-carboxylate

시약·촉매·용매 1

HCID 63651,1-Dichloroethane용매

실험 절차

Combine 2-carboethoxy-4,6-dichloroindole (20.0 g, 0.077 mol), and dimethylformamide (9.0 mL, 0.117 mol) in dichloroethane (100 mL). Add phosphoryl chloride (18.0 g, 0.117 mmol). Heat to reflux. After 3.5 hours, cool the reaction mixture to ambient temperature to obtain a solid. Collect the solid by filtration, rinse with water. Combine the solid with aqueous 1 M sodium acetate solution and stir. After 1 hour, filter, rinse with water, and dry to give 3-formyl-2-carboethoxy-4,6-dichloroindole.

후처리

  1. temperatureHeat to reflux
  2. customto obtain a solid
  3. customCollect the solid
  4. filtrationby filtration
  5. washrinse with water
  6. waitAfter 1 hour
  7. filtrationfilter
  8. washrinse with water
  9. customdry

출처 및 근거

ORD 기록
ord-e04611a419db4adc89247081133ddfb0
출처 데이터셋
uspto-grants-2001_01
특허 번호
US06180786B2

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