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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
ノート
印刷プレビュー

反応式

HRID 1851225 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 3

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒HCID 6344Dichloromethane
溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-4234f3b3989147edbc14156addcf3d16
出典データセット
uspto-grants-2015_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08957064B2

反応ノート

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