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

HRID 1354259
ノート
印刷プレビュー

反応式

HRID 1354259 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 8058Hexane溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-60e50bb4802349689b217cd46ce4d255
出典データセット
uspto-grants-2007_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07223764B2

反応ノート

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