Pyridine → 1-Nitroso-4-(2-thenoyl)piperazine

HRID 1655192ノート

反応式

HRID 1655192 の反応式
[N:1]([N:3]1[CH2:8][CH2:7][NH:6][CH2:5][CH2:4]1)=[O:2].N1C=CC=CC=1.[C:15]1([C:20](Cl)=[O:21])[S:19][CH:18]=[CH:17][CH:16]=1.C(OCC)(=O)C>O1CCOCC1.O>[N:1]([N:3]1[CH2:8][CH2:7][N:6]([C:20](=[O:21])[C:15]2[S:19][CH:18]=[CH:17][CH:16]=2)[CH2:5][CH2:4]1)=[O:2]

参加物

7

反応物 4

HCID 1049PyridineHCID 8857Ethyl AcetateHCID 21845N-NitrosopiperazineHCID 789282-Thiophenecarbonyl chloride

生成物 1

HCID 197912611-Nitroso-4-(2-thenoyl)piperazine

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 312751,4-Dioxane溶媒

実験手順

To a mixture of 1-nitrosopiperazine {1.21 g) and pyridine (2.4 ml) in dioxane (18 ml) was added dropwise 2-thenoyl chloride (1.2 ml) in an ice bath. The mixture was stirred for one hour in an ice.bath and then overnight at ambient temperature. The mixture was poured into a mixture of ethyl acetate (100 ml) and water (100 ml). The separated aqueous layer was extracted twice with ethyl acetate. The combined organic layers were dried and concentrated in vacuo. The residue was pulverized with diisopropyl ether to yield 1-nitroso-4-(2-thenoyl)-piperazine (1.78 g).

後処理

  1. customovernight
  2. customat ambient temperature
  3. extractionThe separated aqueous layer was extracted twice with ethyl acetate
  4. customThe combined organic layers were dried
  5. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-cfc195a29747483781bbdce8c9fc94ce
出典データセット
uspto-grants-1993_10
特許番号
US05250528

反応ノート

読み込み中…