ホームMCPワークベンチSkills
ホームワークベンチ通知マイページ
llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
  1. ホーム
  2. /反応

1-(2-Hydroxyethyl)piperazine → 2-[4-(2-Hydroxyethyl)piperazin-1-yl]-N-[2,4-dibromo-6-methyl-3-pyridyl]acetamide

HRID 348557
ノート
印刷プレビュー

反応式

HRID 348557 の反応式
[Br:1][C:2]1[C:7]([NH:8][C:9](=[O:12])[CH2:10]Br)=[C:6]([Br:13])[CH:5]=[C:4]([CH3:14])[N:3]=1.[OH:15][CH2:16][CH2:17][N:18]1[CH2:23][CH2:22][NH:21][CH2:20][CH2:19]1.C(=O)([O-])[O-].[K+].[K+]>C(#N)C>[Br:1][C:2]1[C:7]([NH:8][C:9](=[O:12])[CH2:10][N:21]2[CH2:22][CH2:23][N:18]([CH2:17][CH2:16][OH:15])[CH2:19][CH2:20]2)=[C:6]([Br:13])[CH:5]=[C:4]([CH3:14])[N:3]=1
参加物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 76771-(2-Hydroxyethyl)piperazineHCID 11430Potassium CarbonateHCID 10430271N-[2,4-dibromo-6-methylpyridin-3-yl]-2-bromoacetamide

生成物 1

HCID 116406602-[4-(2-Hydroxyethyl)piperazin-1-yl]-N-[2,4-dibromo-6-methyl-3-pyridyl]acetamide収率 99%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

N-[2,4-Dibromo-6-methylpyridin-3-yl]-2-bromoacetamide (1.4 g, 37.3 mmol) was dissolved in acetonitrile (60 mL). 1-(2-Hydroxyethyl)piperazine (0.58 g, 4.48 mmol) was added to the solution with stirring and cooling with ice, and then potassium carbonate (37.5 g, 0.271 mol) was added thereto. The temperature of the mixture was elevated to room temperature, and the mixture was stirred for 24 hours. After completion of reaction, the solvent was removed under reduced pressure. Chloroform and water was added to the residue, and the organic layer was collected from the mixture. The aqueous layer was further extracted with chloroform and the two organic layers were combined together. The combined organic layer was washed with saturated brine, dried over sodium sulfate anhydrate, and concentrated under reduced pressure. The residue was purified through silica gel column chromatography (developer: ammonia-saturated methanol/chloroform=1/20), to thereby obtain 1.613 g of N-[2,4-dibromo-6-methylpyridin-3-yl]-2-[4-(2-hydroxyethyl)piperazin-1-yl]acetamide as an amorphous (yield: 99%).

後処理

  1. temperaturecooling with ice
  2. customwas elevated to room temperature
  3. stirringthe mixture was stirred for 24 hours
  4. customAfter completion of reaction
  5. customthe solvent was removed under reduced pressure
  6. additionChloroform and water was added to the residue
  7. customthe organic layer was collected from the mixture
  8. extractionThe aqueous layer was further extracted with chloroform
  9. washThe combined organic layer was washed with saturated brine
  10. dry with materialdried over sodium sulfate anhydrate
  11. concentrationconcentrated under reduced pressure
  12. customThe residue was purified through silica gel column chromatography (developer: ammonia-saturated methanol/chloroform=1/20)

出典と根拠

ORDレコード
ord-4b026e6e1cad481f8a555f17ebac6cdd
出典データセット
uspto-grants-2007_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07176306B2

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート