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

HRID 568185

反応式

HRID 568185 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 63651,1-Dichloroethane溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-e04611a419db4adc89247081133ddfb0
出典データセット
uspto-grants-2001_01
特許番号
US06180786B2

関連ノート

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