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p-Toluenesulfonic acid → HCID 178456629, 화합물

HRID 915014
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인쇄 미리보기

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HRID 915014 반응식
[CH:1]([N:4]1[C:9](=[O:10])[CH:8]=[CH:7][C:6]([C:11](=O)[CH:12]=[N:13][OH:14])=[N:5]1)([CH3:3])[CH3:2].[NH2:16][CH:17]([C:20]#[N:21])[C:18]#[N:19].C1(C)C=CC(S(O)(=O)=O)=CC=1.C([O-])(O)=O.[Na+]>CC(O)C.CCOC(C)=O.O>[NH2:21][C:20]1[C:17]([C:18]#[N:19])=[N:16][C:11]([C:6]2[CH:7]=[CH:8][C:9](=[O:10])[N:4]([CH:1]([CH3:3])[CH3:2])[N:5]=2)=[CH:12][N+:13]=1[O-:14]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 4

HCID 6101p-Toluenesulfonic acidHCID 151258AminomalononitrileHCID 516892Sodium BicarbonateHCID 86600906HCID 86600906, 화합물

생성물 1

HCID 178456629HCID 178456629, 화합물수율 26.4%

시약·촉매·용매 3

HCID 962Water용매
HCID 3776
Isopropanol
용매
HCID 8857Ethyl Acetate용매

반응 조건

온도
50 °C

실험 절차

A mixture of (1-isopropyl-6-oxo-1,6-dihydro-3-pyridazinyl) (oxo)acetaldehyde oxime (11.16 g), aminomalononitrile (13.6 g) and p-toluenesulfonic acid (10.2 g) in 2-propanol (200 ml) was stirred at 50° C. for 3 hours. Water, aq. NaHCO3 and EtOAc were added to the reaction mixture to give a pale yellow precipitate. The precipitate was collected by filtration to obtain 3-amino-6-(1-isopropyl-6-oxo-1,6-dihydro-3-pyridazinyl)-2-pyrazinecarbonitrile 4-oxide (3.84 g) as white powder.

후처리

  1. customto give a pale yellow precipitate
  2. filtrationThe precipitate was collected by filtration

출처 및 근거

ORD 기록
ord-ce5bbd6703154f7a809c9d25a9e25b85
출처 데이터셋
uspto-grants-2007_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07265120B2

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