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

HRID 1350552노트

반응식

HRID 1350552 반응식
[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

참가 물질

3

반응물 1

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

생성물 1

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

시약·촉매·용매 1

HCID 6422Trifluoroacetic acid용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-ff7466892d6a4001bbaba27e64901016
출처 데이터셋
uspto-grants-2007_05
특허 번호
US07214796B2

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