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Pyridine → 6-amino-2-methylpyridazine-3(2H)-thione

HRID 862480
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인쇄 미리보기

반응식

HRID 862480 반응식
N1C=CC=CC=1.COC1C=CC(P2(SP(C3C=CC(OC)=CC=3)(=S)S2)=[S:16])=CC=1.[NH2:29][C:30]1[CH:35]=[CH:34][C:33](=O)[N:32]([CH3:37])[N:31]=1.C(Cl)(Cl)Cl>CO>[NH2:29][C:30]1[CH:35]=[CH:34][C:33](=[S:16])[N:32]([CH3:37])[N:31]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 1049PyridineHCID 6212ChloroformHCID 87949Lawesson's reagentHCID 157119126-Amino-2-methyl-2,3-dihydropyridazin-3-one

생성물 1

HCID 196983986-amino-2-methylpyridazine-3(2H)-thione수율 64.3%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

Pyridine (5 ml) and a Lawesson's reagent (970 mg, 2.4 mmol) were added to 3-amino-1-methyl-1,6-dihydropyridazin-6-one (500 mg, 4 mmol) as described in Journal of Medicinal Chemistry, 34 (10), 3074 (1991), and the mixture was refluxed under heating for 5 hours. The reaction mixture was concentrated and the residue obtained was subjected to silica gel column chromatography (chloroform:methanol=100:1) to give 218 mg of 3-amino-1-methyl-1,6-dihydropyridazine-6-thione.

후처리

  1. temperaturethe mixture was refluxed
  2. temperatureunder heating for 5 hours
  3. concentrationThe reaction mixture was concentrated
  4. customthe residue obtained

출처 및 근거

ORD 기록
ord-8669ca35e835445da07adb346df577bd
출처 데이터셋
uspto-grants-1998_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05719155

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