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2,5-Dibromopyridine → 1-(5-Bromopyridin-2-yl)-4-isopropylpiperazine

HRID 1726876
ノート
印刷プレビュー

反応式

HRID 1726876 の反応式
Br[C:2]1[CH:7]=[CH:6][C:5]([Br:8])=[CH:4][N:3]=1.[CH:9]([N:12]1[CH2:17][CH2:16][NH:15][CH2:14][CH2:13]1)([CH3:11])[CH3:10].C1CCN2C(=NCCC2)CC1>O>[Br:8][C:5]1[CH:6]=[CH:7][C:2]([N:15]2[CH2:16][CH2:17][N:12]([CH:9]([CH3:11])[CH3:10])[CH2:13][CH2:14]2)=[N:3][CH:4]=1
参加物反応条件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 693532,5-DibromopyridineHCID 780131-IsopropylpiperazineHCID 811841,8-Diazabicyclo(5.4.0)undec-7-ene

生成物 1

HCID 199958461-(5-Bromopyridin-2-yl)-4-isopropylpiperazine

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
100 °C

実験手順

A solution containing 12.1 g of 2,5-dibromopyridine (51.1 mmol), 8.8 ml of 1-isopropyl-piperazine (61.5 mmol) and 9.2 ml of DBU (61.5 mmol) is stirred overnight at 100° C. The reaction mixture is returned to ambient temperature and the solution is diluted with water and extracted with ethyl acetate. The organic phases are collected, washed with brine, dried (MgSO4) and evaporated under reduced pressure. The residue is chromatographed on an SiO2 column, eluting with a mixture of CH2Cl2/MeOH 98/2 and then 96/4, to yield the title product.

後処理

  1. customis returned to ambient temperature
  2. extractionextracted with ethyl acetate
  3. customThe organic phases are collected
  4. washwashed with brine
  5. dry with materialdried (MgSO4)
  6. customevaporated under reduced pressure
  7. customThe residue is chromatographed on an SiO2 column
  8. washeluting with a mixture of CH2Cl2/MeOH 98/2

出典と根拠

ORDレコード
ord-66071ff33a8547aba107ea3a9d37c801
出典データセット
uspto-grants-2009_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07494994B2

反応ノート

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このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート