Water → 1-(5-Bromopyridin-2-yl)piperazine

HRID 80914

반응식

HRID 80914 반응식
[NH:1]1[CH2:6][CH2:5][NH:4][CH2:3][CH2:2]1.Cl[C:8]1[CH:13]=[CH:12][C:11]([Br:14])=[CH:10][N:9]=1.O>C1(C)C=CC=CC=1>[Br:14][C:11]1[CH:12]=[CH:13][C:8]([N:1]2[CH2:6][CH2:5][NH:4][CH2:3][CH2:2]2)=[N:9][CH:10]=1

참가 물질

5

반응물 3

HCID 962WaterHCID 4837PiperazineHCID 27344145-Bromo-2-chloropyridine

생성물 1

HCID 164142271-(5-Bromopyridin-2-yl)piperazine수율 80%

시약·촉매·용매 1

HCID 1140Toluene용매2회

반응 조건

온도
130 °C

실험 절차

A mixture of piperazine (107 g, 1.24 mol) and 2-chloro-5-bromopyridine (30 g, 156 mmol) in toluene (150 mL) was heated at 130° C. for 2 hours, The reaction mixture was cooled to room temperature and toluene (400 mL) and water (200 mL) were added. The organic phase was isolated and the aqeuous phase was extracted once with toluene (100 mL). The collected organic phases were washed with water (150 mL) and brine (100 mL), dried over magnesium sulphate and evaporated to dryness in vacuo to give 30.1 g (80%) of 1-(5-bromopyridin-2-yl)-piperazine.

후처리

  1. temperatureThe reaction mixture was cooled to room temperature
  2. customThe organic phase was isolated
  3. extractionthe aqeuous phase was extracted once with toluene (100 mL)
  4. washThe collected organic phases were washed with water (150 mL) and brine (100 mL)
  5. dry with materialdried over magnesium sulphate
  6. customevaporated to dryness in vacuo

출처 및 근거

ORD 기록
ord-7891133c7fb9466eab26c0967f32c960
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08846677B2

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