1-[2-(Benzimidazol-2-ylthio)ethyl]-4-tert-butoxycarbonyl piperazine → 1-[2-(Benzimidazol-2-ylthio)ethyl]piperazine

HRID 1350552ノート

反応式

HRID 1350552 の反応式
[N:1]1[C:5]2[CH:6]=[CH:7][CH:8]=[CH:9][C:4]=2[NH:3][C:2]=1[S:10][CH2:11][CH2:12][N:13]1[CH2:18][CH2:17][N:16](C(OC(C)(C)C)=O)[CH2:15][CH2:14]1>FC(F)(F)C(O)=O>[N:1]1[C:5]2[CH:6]=[CH:7][CH:8]=[CH:9][C:4]=2[NH:3][C:2]=1[S:10][CH2:11][CH2:12][N:13]1[CH2:18][CH2:17][NH:16][CH2:15][CH2:14]1

参加物

3

反応物 1

HCID 230848911-[2-(Benzimidazol-2-ylthio)ethyl]-4-tert-butoxycarbonyl piperazine

生成物 1

HCID 99617871-[2-(Benzimidazol-2-ylthio)ethyl]piperazine収率 152.3%

試薬・触媒・溶媒 1

HCID 6422Trifluoroacetic acid溶媒

実験手順

1-[2-(benzimidazol-2-ylthio)ethyl]-4-tert-butoxycarbonyl piperazine (13.83 g, 38.15 mmol) was dissolved in trifluoroacetic acid (75 mL) in an ice bath, and the mixture was stirred at the same temperature for 30 minutes, and after elevating the temperature to room temperature, the mixture was stirred for another 40 minutes. The reaction solution was concentrated under reduced pressure, and the resulting crystals were recrystallized from methanol-diethyether to give 15.24 g of 1-[2-(benzimidazole-2-ylthio)ethyl]piperazine.3 trifluoroacetate (66%) as pale yellow powdery crystals.

後処理

  1. customto room temperature
  2. stirringthe mixture was stirred for another 40 minutes
  3. concentrationThe reaction solution was concentrated under reduced pressure
  4. customthe resulting crystals were recrystallized from methanol-diethyether

出典と根拠

ORDレコード
ord-ff7466892d6a4001bbaba27e64901016
出典データセット
uspto-grants-2007_05
特許番号
US07214796B2

反応ノート

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