Thionyl Chloride → HCID 59436266, 화합물

HRID 1895089노트

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HRID 1895089 반응식
[O:1]=[C:2]1[CH:7]=[CH:6][N:5]([C:8]2[CH:13]=[CH:12][CH:11]=[C:10]([C:14]([F:17])([F:16])[F:15])[CH:9]=2)[N:4]=[C:3]1[C:18]([NH:20][C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1)=O.[NH:27]1[C:31]2[CH:32]=[CH:33][CH:34]=[CH:35][C:30]=2[N:29]=[N:28]1.S(Cl)(Cl)=O>C(Cl)Cl>[N:27]1([C:18](=[N:20][C:21]2[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=2)[C:3]2[C:2](=[O:1])[CH:7]=[CH:6][N:5]([C:8]3[CH:13]=[CH:12][CH:11]=[C:10]([C:14]([F:17])([F:15])[F:16])[CH:9]=3)[N:4]=2)[C:31]2[CH:32]=[CH:33][CH:34]=[CH:35][C:30]=2[N:29]=[N:28]1

참가 물질

5

반응물 3

HCID 24386Thionyl ChlorideHCID 1481283HCID 1481283, 화합물HCID 178418385HCID 178418385, 화합물

생성물 1

HCID 59436266HCID 59436266, 화합물수율 58.1%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

A solution of 4-oxo-N-phenyl-1-[3-(trifluoromethyl)phenyl]-1,4-dihydropyridazine-3-carboxamide (0.153 g, 0.426 mmol), 1H-benzo[d][1,2,3]triazole (0.201 g, 1.69 mmol) and thionyl chloride (0.06 mL, 0.82 mmol) in methylene chloride (2 mL) was heated under microwave heating conditions at 80 watts of power for 10 min. After that time, the reaction was concentrated and the crude product purified by flash column chromatography (silica gel, hexanes to ethyl acetate) to give 0.114 g (58%) of 3-[1H-benzotriazol-1-yl(phenylimino)methyl]-1-[3-(trifluoromethyl)phenyl]pyridazin-4(1H)-one as a pale red solid that was used without further characterization.

후처리

  1. temperatureheating conditions at 80 watts of power for 10 min
  2. concentrationAfter that time, the reaction was concentrated
  3. customthe crude product purified by flash column chromatography (silica gel, hexanes to ethyl acetate)

출처 및 근거

ORD 기록
ord-41ab349bc7ed430d826ca4a6d5e6f10c
출처 데이터셋
uspto-grants-2013_08
특허 번호
US08513251B2

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