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Diethyl Ether → 1-[2-(5-Fluorobenzimidazol-2-ylthio)ethyl]piperazine tris(trifluoroacetic acid) salt

HRID 1354259
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HRID 1354259 반응식
[F:1][C:2]([F:7])([F:6])[C:3]([OH:5])=[O:4].C(OC([N:15]1[CH2:20][CH2:19][N:18]([CH2:21][CH2:22][S:23][C:24]2[NH:25][C:26]3[CH:32]=[C:31]([F:33])[CH:30]=[CH:29][C:27]=3[N:28]=2)[CH2:17][CH2:16]1)=O)(C)(C)C.CCOCC>CCCCCC>[F:1][C:2]([F:7])([F:6])[C:3]([OH:5])=[O:4].[F:1][C:2]([F:7])([F:6])[C:3]([OH:5])=[O:4].[F:1][C:2]([F:7])([F:6])[C:3]([OH:5])=[O:4].[F:33][C:31]1[CH:30]=[CH:29][C:27]2[N:28]=[C:24]([S:23][CH2:22][CH2:21][N:18]3[CH2:19][CH2:20][NH:15][CH2:16][CH2:17]3)[NH:25][C:26]=2[CH:32]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 3283Diethyl EtherHCID 6422Trifluoroacetic acidHCID 231161621-Tert-butoxycarbonyl-4-[2-(5-fluorobenzimidazol-2-ylthio)ethyl]piperazine

생성물 1

HCID 231161601-[2-(5-Fluorobenzimidazol-2-ylthio)ethyl]piperazine tris(trifluoroacetic acid) salt수율 99%

시약·촉매·용매 1

HCID 8058Hexane용매

실험 절차

While trifluoroacetic acid (17 mL) was stirred under cooling with ice, 1-tert-butoxycarbonyl-4-[2-(5-fluorobenzimidazol-2-ylthio)ethyl]piperazine (6.50 g, 17.08 mmol) was added to the acid over 30 minutes and dissolved thereto. The temperature of the mixture was allowed to room temperature, and the mixture was stirred for 30 minutes. Thereafter, ether and hexane were added thereto, and the formed solid was collected through filtration. The collected product was washed with ether, to thereby yield 1-[2-(5-fluorobenzimidazol-2-ylthio)ethyl]piperazine tris(trifluoroacetic acid) salt (10.50 g, yield 99%) as a brown powder.

후처리

  1. additionwas added to the acid over 30 minutes
  2. dissolutiondissolved
  3. customwas allowed to room temperature
  4. filtrationthe formed solid was collected through filtration
  5. washThe collected product was washed with ether

출처 및 근거

ORD 기록
ord-60e50bb4802349689b217cd46ce4d255
출처 데이터셋
uspto-grants-2007_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07223764B2

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