Hydrochloric Acid → N-ethyl-2,5-difluoro-4-(piperazin-1-yl)benzamide hydrochloride

HRID 69721노트

반응식

HRID 69721 반응식
[CH2:1]([NH:3][C:4]([C:6]1[C:11]([F:12])=[CH:10][C:9]([N:13]2[CH2:18][CH2:17][N:16](C(OC(C)(C)C)=O)[CH2:15][CH2:14]2)=[C:8]([F:26])[CH:7]=1)=[O:5])[CH3:2].[ClH:27]>O1CCOCC1.C(OCC)C>[ClH:27].[CH2:1]([NH:3][C:4](=[O:5])[C:6]1[CH:7]=[C:8]([F:26])[C:9]([N:13]2[CH2:18][CH2:17][NH:16][CH2:15][CH2:14]2)=[CH:10][C:11]=1[F:12])[CH3:2]

참가 물질

5

반응물 2

HCID 313Hydrochloric AcidHCID 58324386HCID 58324386, 화합물

생성물 1

HCID 66775087N-ethyl-2,5-difluoro-4-(piperazin-1-yl)benzamide hydrochloride수율 98%

시약·촉매·용매 2

HCID 3283Diethyl Ether용매HCID 312751,4-Dioxane용매

실험 절차

tert-butyl 4-(4-(ethylcarbamoyl)-2,5-difluorophenyl)piperazine-1-carboxylate (0.020 g, 0.054 mmol) was diluted with 4.0M HCl in dioxane (3 mL) and stirred for 30 min. The thick white precipitate that formed was diluted with ethyl ether (10 mL) and stirred until a fine suspension resulted. The precipitate was filtered under nitrogen and dried in vacuum to afford N-ethyl-2,5-difluoro-4-(piperazin-1-yl)benzamide hydrochloride (16.2 mg, 0.053 mmol, 98% yield) as a white solid. ESI-MS: m/z 270 (M+H)+.

후처리

  1. customThe thick white precipitate that formed
  2. stirringstirred until a fine suspension
  3. customresulted
  4. filtrationThe precipitate was filtered under nitrogen
  5. customdried in vacuum

출처 및 근거

ORD 기록
ord-31b9e865114e448eb5216315d9759073
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08822470B2

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