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3-bromo-2-chloro-5-(4-ethylpiperazin-1-ylsulfonyl)pyridine → HCID 22052242、化合物

HRID 2305411
ノート
印刷プレビュー

反応式

HRID 2305411 の反応式
[Br:1][C:2]1[C:3](Cl)=[N:4][CH:5]=[C:6]([S:8]([N:11]2[CH2:16][CH2:15][N:14]([CH2:17][CH3:18])[CH2:13][CH2:12]2)(=[O:10])=[O:9])[CH:7]=1.[O-:20][CH2:21][CH3:22].[Na+]>C(O)C>[Br:1][C:2]1[C:3]([O:20][CH2:21][CH3:22])=[N:4][CH:5]=[C:6]([S:8]([N:11]2[CH2:16][CH2:15][N:14]([CH2:17][CH3:18])[CH2:13][CH2:12]2)(=[O:10])=[O:9])[CH:7]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 10342243-bromo-2-chloro-5-(4-ethylpiperazin-1-ylsulfonyl)pyridineHCID 2723922Sodium ethoxide

生成物 1

HCID 22052242HCID 22052242、化合物収率 95%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A mixture of 3-bromo-2-chloro-5-(4-ethylpiperazin-1-ylsulfonyl)pyridine (Preparation 9; 6.60 g, 17.9 mmol) and sodium ethoxide (6.09 g, 89.55 mmol) in ethanol (100 mL) was heated under reflux for 18 hours, then cooled. The reaction mixture was concentrated under reduced pressure, the residue partitioned between water (100 mL) and ethyl acetate (100 mL), and the layers separated. The aqueous phase was extracted with ethyl acetate (2×100 mL), the combined organic solutions dried (MgSO4) and evaporated under reduced pressure to afford the title compound as a brown solid (6.41 g, 95%).

後処理

  1. temperaturewas heated
  2. temperatureunder reflux for 18 hours
  3. temperaturecooled
  4. concentrationThe reaction mixture was concentrated under reduced pressure
  5. customthe residue partitioned between water (100 mL) and ethyl acetate (100 mL)
  6. customthe layers separated
  7. extractionThe aqueous phase was extracted with ethyl acetate (2×100 mL)
  8. dry with materialthe combined organic solutions dried (MgSO4)
  9. customevaporated under reduced pressure

出典と根拠

ORDレコード
ord-8c963473a5274bc3ba83dea197e1b3a1
出典データセット
uspto-grants-2002_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06440982B1

反応ノート

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