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Dimethylamine → 5-Chloro-N,N,2-trimethyl-6-phenyl[1,2,4]triazolo[1,5-a]pyrimidin-7-amine

HRID 1851225
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HRID 1851225 반응식
[Cl:1][C:2]1[C:7]([C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)=[C:6](Cl)[N:5]2[N:15]=[C:16]([CH3:18])[N:17]=[C:4]2[N:3]=1.[CH3:19][NH:20][CH3:21]>CN(C=O)C.O.ClCCl>[Cl:1][C:2]1[C:7]([C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)=[C:6]([N:20]([CH3:21])[CH3:19])[N:5]2[N:15]=[C:16]([CH3:18])[N:17]=[C:4]2[N:3]=1
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참가 물질

6

반응물 2

HCID 674DimethylamineHCID 866306805,7-Dichloro-2-methyl-6-phenyl[1,2,4]triazolo[1,5-a]pyrimidine

생성물 1

HCID 866306975-Chloro-N,N,2-trimethyl-6-phenyl[1,2,4]triazolo[1,5-a]pyrimidin-7-amine

시약·촉매·용매 3

HCID 962Water용매HCID 6228Dimethylformamide용매HCID 6344
Dichloromethane
용매

실험 절차

To 500 mg 5,7-dichloro-2-methyl-6-phenyl[1,2,4]triazolo[1,5-a]pyrimidine (prepared as described above) in 25 mL DMF were added 0.8 mL of a dimethylamine solution (60% in water). The mixture was stirred at room temperature for 45 minutes. The reaction mixture was diluted with water and dichloromethane. The phases were separated and the water layer was extracted with dichloromethane. The combined organic layers were dried over Na2SO4 and the solvent was removed by evaporation. The residue was suspended in diethylether and stirred for 5 hours. The desired product was filtered, dried and was used without further purification for the next step.

후처리

  1. customThe phases were separated
  2. extractionthe water layer was extracted with dichloromethane
  3. dry with materialThe combined organic layers were dried over Na2SO4
  4. customthe solvent was removed by evaporation
  5. stirringstirred for 5 hours
  6. filtrationThe desired product was filtered
  7. customdried
  8. customwas used without further purification for the next step

출처 및 근거

ORD 기록
ord-4234f3b3989147edbc14156addcf3d16
출처 데이터셋
uspto-grants-2015_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08957064B2

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