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Ammonia → 5-Chloro-2-methyl-6-phenyl[1,2,4]triazolo[1,5-a]pyrimidine

HRID 503768
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HRID 503768 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.N>ClCCl.[Cl-].[Na+].O.[Zn]>[Cl:1][C:2]1[C:7]([C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)=[CH:6][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 222AmmoniaHCID 866306805,7-Dichloro-2-methyl-6-phenyl[1,2,4]triazolo[1,5-a]pyrimidine

생성물 1

HCID 772315025-Chloro-2-methyl-6-phenyl[1,2,4]triazolo[1,5-a]pyrimidine

시약·촉매·용매 3

HCID 23994Zinc촉매HCID 6344Dichloromethane용매HCID 57417360Sodium chloride; water
용매

실험 절차

34.5 g 5,7-dichloro-2-methyl-6-phenyl[1,2,4]triazolo[1,5-a]pyrimidine is dissolved in 500 ml dichloromethane. 500 ml brine, 250 ml ammonia solution 25% w/w and 34.0 g zinc powder are added and the mixture is stirred at room temperature for 1 h. The reaction mixture is filtrated over kieselgur and is washed with dichloromethane and water. The organic phase is separated and the water phase is extracted with dichloromethane. The combined dichloromethane phase is dried over Na2SO4 and the solvent is evaporated. The crude product is purified by chromatography on silica gel (dichloromethane/ethyl acetate) to yield the desired compound.

후처리

  1. filtrationThe reaction mixture is filtrated over kieselgur
  2. washis washed with dichloromethane and water
  3. customThe organic phase is separated
  4. extractionthe water phase is extracted with dichloromethane
  5. dry with materialThe combined dichloromethane phase is dried over Na2SO4
  6. customthe solvent is evaporated
  7. customThe crude product is purified by chromatography on silica gel (dichloromethane/ethyl acetate)

출처 및 근거

ORD 기록
ord-aa19a5d6941d48289adae1f9196032b0
출처 데이터셋
uspto-grants-2010_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07776864B2

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