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Dimethyl Sulfoxide → HCID 21464366, 화합물

HRID 1940929
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HRID 1940929 반응식
CS(C)=O.Cl[S:6]([C:9]1[N:20]=[C:12]2[C:13]([O:18][CH3:19])=[CH:14][CH:15]=[C:16]([Cl:17])[N:11]2[N:10]=1)(=[O:8])=[O:7].[F:21][C:22]1[CH:28]=[CH:27][CH:26]=[C:25]([F:29])[C:23]=1[NH2:24].N1C=CC=CC=1>C(#N)C.O.ClCCl>[F:21][C:22]1[CH:28]=[CH:27][CH:26]=[C:25]([F:29])[C:23]=1[NH:24][S:6]([C:9]1[N:20]=[C:12]2[C:13]([O:18][CH3:19])=[CH:14][CH:15]=[C:16]([Cl:17])[N:11]2[N:10]=1)(=[O:8])=[O:7]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 4

HCID 679Dimethyl SulfoxideHCID 1049PyridineHCID 796472,6-DifluoroanilineHCID 21464365HCID 21464365, 화합물

생성물 1

HCID 21464366HCID 21464366, 화합물수율 62.3%

시약·촉매·용매 3

HCID 962Water용매
HCID 6342
Acetonitrile
용매
HCID 6344Dichloromethane용매

실험 절차

Dimethyl sulfoxide (90 microliters, 94 micrograms, 1.2 mmol) was added with stirring to a solution of 2-chlorosulfonyl-5-chloro-8-methoxy[1,2,4]triazolo[1,5-a]pyridine (1.7 g, 6 mmol), 2,6-difluoroaniline (1.6 g, 12 mmol) and pyridine (0.5 g, 6 mmol) in acetonitrile (20 mL) at ambient temperature. The reaction was complete in about 20 min. Dichloromethane and water were added and the solid that separated was collected by filtration. The organic layer was concentrated by evaporation and the residue obtained was washed with water and combined with the earlier obtained solid. The combined solids were then washed with ether and hexane and dried to obtain 1.4 g of the title compound as an off-white powder melting at 190°-191° C. (d).

후처리

  1. customthe solid that separated
  2. filtrationwas collected by filtration
  3. concentrationThe organic layer was concentrated by evaporation
  4. customthe residue obtained
  5. washwas washed with water
  6. customearlier obtained solid
  7. washThe combined solids were then washed with ether and hexane
  8. customdried

출처 및 근거

ORD 기록
ord-d6a20e1085c84032b6361399916057f6
출처 데이터셋
uspto-grants-1997_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05700940

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