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Hydrochloric Acid → 1H-Benzimidazole, 5,6-difluoro-2-[[2-(1-piperazinyl)ethyl]thio]-

HRID 1354253
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HRID 1354253 반응식
[F:1][C:2]1[C:21]([F:22])=[CH:20][C:5]2[N:6]=[C:7]([S:9][CH2:10][CH2:11][N:12]3[CH2:17][CH2:16][N:15](C=O)[CH2:14][CH2:13]3)[NH:8][C:4]=2[CH:3]=1.Cl>CO>[F:1][C:2]1[C:21]([F:22])=[CH:20][C:5]2[N:6]=[C:7]([S:9][CH2:10][CH2:11][N:12]3[CH2:17][CH2:16][NH:15][CH2:14][CH2:13]3)[NH:8][C:4]=2[CH:3]=1
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참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 231161611-[2-(5,6-Difluorobenzimidazol-2-ylthio)ethyl]-4-formylpiperazine

생성물 1

HCID 115222491H-Benzimidazole, 5,6-difluoro-2-[[2-(1-piperazinyl)ethyl]thio]-수율 90.2%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

1-[2-(5,6-Difluorobenzimidazol-2-ylthio)ethyl]-4-formylpiperazine (1.70 g, 5.2 mmol) was dissolved in methanol (20 mL), and 12N hydrochloric acid (2 mL) was added to the solution, followed by stirring for 18 hours at room temperature. The reaction mixture was concentrated under reduced pressure, and saturated ammonia-methanol was added thereto, followed by stirring for five minutes at room temperature. The solvent was removed under reduced pressure, and the residue was purified through silica gel column chromatography (chloroform: saturated ammonia-methanol=100:3), to thereby yield 1-[2-(5,6-difluorobenzimidazol-2-ylthio)ethyl]piperazine (1.40 g, yield 90%) as a brown oil.

후처리

  1. concentrationThe reaction mixture was concentrated under reduced pressure, and saturated ammonia-methanol
  2. additionwas added
  3. stirringby stirring for five minutes at room temperature
  4. customThe solvent was removed under reduced pressure
  5. customthe residue was purified through silica gel column chromatography (chloroform: saturated ammonia-methanol=100:3)

출처 및 근거

ORD 기록
ord-81c3da7ab46f46ccbc46531ceb38700a
출처 데이터셋
uspto-grants-2007_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07223764B2

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