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Hydrochloric Acid → 4-bromo-1-methyl-1H-pyrrole-2-carboxylic acid amide

HRID 1025576
ノート
印刷プレビュー

反応式

HRID 1025576 の反応式
[Br:1][C:2]1[CH:3]=[C:4]([C:8](=[O:13])C(F)(F)F)[N:5]([CH3:7])[CH:6]=1.Cl.[OH-].[NH4+:16]>>[Br:1][C:2]1[CH:3]=[C:4]([C:8]([NH2:16])=[O:13])[N:5]([CH3:7])[CH:6]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 3

HCID 313Hydrochloric AcidHCID 14923Ammonium HydroxideHCID 710083441-(4-bromo-1-methyl-1H-pyrrol-2-yl)-2,2,2-trifluoroethanone

生成物 1

HCID 434111534-bromo-1-methyl-1H-pyrrole-2-carboxylic acid amide収率 81%

実験手順

1-(4-bromo-1-methyl-1H-pyrrol-2-yl)-2,2,2-trifluoroethanone (5.0 g, 19.5 mmol) was dissolved in ammonium hydroxide (72.5 ml, 29.4% aqueous solution) and stirred at room temperature for 45 min. The solution was brought to pH=7 with 2N HCl. The solid precipitate was collected by filtration. The solid was washed with water and dried overnight under reduced pressure at 50° C. The aqueous layer was extracted twice with dichloromethane. The organic phase was concentrated in vacuo to afford more solid. Solid from the filtration and extraction were combined to afford 4-bromo-1-methyl-1H-pyrrole-2-carboxylic acid amide (3.2 g, 81%) as a white solid: LC/MS-ESI observed [M+H]+ 203 and 205.

このページの内容参加物実験手順後処理出典と根拠反応ノート

後処理

  1. filtrationThe solid precipitate was collected by filtration
  2. washThe solid was washed with water
  3. customdried overnight under reduced pressure at 50° C
  4. extractionThe aqueous layer was extracted twice with dichloromethane
  5. concentrationThe organic phase was concentrated in vacuo
  6. customto afford more solid
  7. filtrationSolid from the filtration and extraction

出典と根拠

ORDレコード
ord-ff70da8183334821a0c211dd8a59e17b
出典データセット
uspto-grants-2014_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08729078B2

反応ノート

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