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

HRID 1655192노트

반응식

HRID 1655192 반응식
[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]

참가 물질

7

반응물 4

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

생성물 1

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

시약·촉매·용매 2

HCID 962Water용매HCID 312751,4-Dioxane용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-cfc195a29747483781bbdce8c9fc94ce
출처 데이터셋
uspto-grants-1993_10
특허 번호
US05250528

반응 노트

불러오는 중…