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Pyridine → 5-Chloro-3-iodo-1H-pyrrolo[2,3-b]pyridine

HRID 1396130
ノート
印刷プレビュー

反応式

HRID 1396130 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]2[CH:10]=[CH:9][NH:8][C:5]2=[N:6][CH:7]=1.N1C=CC=CC=1.[I:17]Cl>ClCCl>[Cl:1][C:2]1[CH:3]=[C:4]2[C:10]([I:17])=[CH:9][NH:8][C:5]2=[N:6][CH:7]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 1049PyridineHCID 24640Iodine chlorideHCID 242292135-Chloro-1H-pyrrolo[2,3-b]pyridine

生成物 1

HCID 242292205-Chloro-3-iodo-1H-pyrrolo[2,3-b]pyridine

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a solution of 5-chloro-1H-pyrrolo[2,3-b]pyridine (1, 15.00 g, 98.31 mmol) in 300 mL of dichloromethane under an atmosphere or nitrogen, pyridine (7.951 mL, 98.31 mmol) and iodine monochloride (110 mL, 1.0 M in dichloromethane, 110 mmol) are added slowly over 20 minutes. The reaction is stirred at room temperature for 2 hours, then quenched with 100 mL of 1 M aqueous sodium thiosulfate pentahydrate. The layers are separated, solids collected from the aqueous layer by filtration and combined with the organic layer. The aqueous layer is extracted with ethyl acetate, and the organic layers are combined and washed with brine, then concentrated under vacuum. The resulting solid is washed with 20% ethyl acetate in hexane to provide the desired compound.

後処理

  1. customquenched with 100 mL of 1 M aqueous sodium thiosulfate pentahydrate
  2. customThe layers are separated
  3. filtrationsolids collected from the aqueous layer by filtration
  4. extractionThe aqueous layer is extracted with ethyl acetate
  5. washwashed with brine
  6. concentrationconcentrated under vacuum
  7. washThe resulting solid is washed with 20% ethyl acetate in hexane

出典と根拠

ORDレコード
ord-ab3cbc7676364e108e7e86bf5829968e
出典データセット
uspto-grants-2014_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08901118B2

反応ノート

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