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

HRID 1025576
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HRID 1025576 반응식
[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
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 3

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

생성물 1

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

실험 절차

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.

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후처리

  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

출처 및 근거

ORD 기록
ord-ff70da8183334821a0c211dd8a59e17b
출처 데이터셋
uspto-grants-2014_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08729078B2

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