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

Piperazine → HCID 10982183、化合物

HRID 1603587
ノート
印刷プレビュー

反応式

HRID 1603587 の反応式
Br[C:2]1[CH:7]=[C:6]([S:8]([C:11]2[CH:16]=[CH:15][C:14]([NH2:17])=[CH:13][CH:12]=2)(=[O:10])=[O:9])[CH:5]=[C:4]([Br:18])[N:3]=1.[NH:19]1[CH2:24][CH2:23][NH:22][CH2:21][CH2:20]1.C(N(CC)CC)C>O1CCOCC1>[Br:18][C:4]1[CH:5]=[C:6]([S:8]([C:11]2[CH:16]=[CH:15][C:14]([NH2:17])=[CH:13][CH:12]=2)(=[O:10])=[O:9])[CH:7]=[C:2]([N:19]2[CH2:24][CH2:23][NH:22][CH2:21][CH2:20]2)[N:3]=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 4837PiperazineHCID 8471TriethylamineHCID 110146744-[(2,6-Dibromo-4-pyridinyl)sulfonyl]aniline

生成物 1

HCID 10982183HCID 10982183、化合物収率 82.7%

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

反応条件

温度
40 °C

実験手順

0.275 g (0.0007 mol) of 4-(2,6-dibromopyridine-4-sulphonyl)-phenylamine was dissolved in 10 ml of dioxane and treated with 0.066 g (0.00077 mol) of piperazine and 1 ml of triethylamine. The mixture was stirred at 40° C. for 72 hrs. and the solvent was then removed. The residue was partitioned in ethyl acetate and water and the organic phase was extracted with sat. sodium chloride solution and dried over MgSO4 and filtered. After removal of the solvent the residue was chromatographed on silica gel with dichloromethane/methanol 9:1 and there was obtained 0.23 g (82%) of 4-(2-bromo-6-piperazin-1-ylpyridin-4-sulphonyl) -phenylamine as yellowish crystals; m.p.: 173-175° C.

後処理

  1. customand the solvent was then removed
  2. customThe residue was partitioned in ethyl acetate
  3. extractionwater and the organic phase was extracted with sat. sodium chloride solution
  4. dry with materialdried over MgSO4
  5. filtrationfiltered
  6. customAfter removal of the solvent the residue
  7. customwas chromatographed on silica gel with dichloromethane/methanol 9:1

出典と根拠

ORDレコード
ord-1f8bb73f991f4c5bb070ff7f5bddebe2
出典データセット
uspto-grants-1999_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05990105

反応ノート

読み込み中…

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