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Hydrochloric Acid → HCID 86704560、化合物

HRID 1022430
ノート
印刷プレビュー

反応式

HRID 1022430 の反応式
Cl[C:2]1[C:7]2[CH:8]=[CH:9][N:10]([CH2:11][CH3:12])[C:6]=2[CH:5]=[C:4]([Cl:13])[N:3]=1.[OH-:14].[Na+].Cl>O1CCOCC1>[Cl:13][C:4]1[NH:3][C:2](=[O:14])[C:7]2[CH:8]=[CH:9][N:10]([CH2:11][CH3:12])[C:6]=2[CH:5]=1
参加物反応条件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 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 86704559HCID 86704559、化合物

生成物 1

HCID 86704560HCID 86704560、化合物収率 32.8%

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

反応条件

温度
160 °C

実験手順

A microwave reaction vial was charged with 4,6-dichloro-1-ethyl-1H-pyrrolo[3,2-c]pyridine (200 mg, 0.930 mmol), a 2M aqueous sodium hydroxide solution (10 mL) and 1,4-dioxane (3 mL). The vial was sealed and then heated in the microwave at 160° C. for 30 min. At this time, the resulting mixture was acidified to pH 6.5 with a 4M aqueous hydrochloric acid solution and then concentrated in vacuo. The residue was diluted with ethanol. The solids were removed by filtration, and the filtrate was concentrated in vacuo. Flash chromatography (10/1 methylene chloride/methanol) afforded 6-chloro-1-ethyl-1,5-dihydro-pyrrolo[3,2-c]pyridine-4-one (60 mg, 32.8%). LC-MS calcd. for C9H9ClN2O [(M)+] 196, obsd. 196.9.

後処理

  1. customA microwave reaction
  2. customThe vial was sealed
  3. concentrationconcentrated in vacuo
  4. additionThe residue was diluted with ethanol
  5. customThe solids were removed by filtration
  6. concentrationthe filtrate was concentrated in vacuo

出典と根拠

ORDレコード
ord-7f3b7028ac86409e9095ea7037dc20bd
出典データセット
uspto-grants-2014_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08722661B2

反応ノート

読み込み中…

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