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

HRID 503800
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HRID 503800 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 under example 37) in 25 ml DMF are added 0.8 ml of a dimethylamin solution (60% in water). The mixture is stirred at room temperature for 45 minutes. The reaction mixture is diluted with water and dichloromethane. The phases are separated and the water layer is extracted with dichloromethane. The combined organic layers are dried over Na2SO4 and the solvent is removed by evaporation. The residue is suspended in diethylether and stirred for 5 hours. The desired product is filtered, dried and is used without further purification for the next step.

후처리

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

출처 및 근거

ORD 기록
ord-0d017a7490754d5793d5dca564f939b7
출처 데이터셋
uspto-grants-2010_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07776864B2

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