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Ammonia → 2,4-Diamino-6-methyl-5-(2,3,5-trichloro-4-nitrophenyl)pyrimidine

HRID 846357
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HRID 846357 반응식
[NH2:1][C:2]1[N:7]=[C:6]([NH2:8])[C:5]([C:9]2[CH:14]=[C:13]([Cl:15])[CH:12]=[C:11]([Cl:16])[C:10]=2[Cl:17])=[C:4]([CH3:18])[N:3]=1.[N+:19]([O-])([O-:21])=[O:20].[K+].N>S(=O)(=O)(O)O>[NH2:1][C:2]1[N:7]=[C:6]([NH2:8])[C:5]([C:9]2[CH:14]=[C:13]([Cl:15])[C:12]([N+:19]([O-:21])=[O:20])=[C:11]([Cl:16])[C:10]=2[Cl:17])=[C:4]([CH3:18])[N:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 222AmmoniaHCID 24434Potassium NitrateHCID 115512322,4-Diamino-6-methyl-5-(2,3,5-trichlorophenyl)pyrimidine

생성물 1

HCID 233535442,4-Diamino-6-methyl-5-(2,3,5-trichloro-4-nitrophenyl)pyrimidine

시약·촉매·용매 1

HCID 1118Sulfuric Acid용매

실험 절차

2,4-Diamino-6-methyl-5-(2,3,5-trichlorophenyl)pyrimidine (0.152 g) (Example 6) was dissolved in concentrated sulphuric acid and potassium nitrate (50 mg) was added. The solution was stirred at room temperature overnight, then poured onto ice and basified with 0.880 ammonia. The product was extracted into ethyl acetate, bulked, dried (MgSO4) and evaporated. The residue was purified by chromatography on SiO2 gel, eluting with EtOAc to 8% MeOH/EtOAc to give the desired product, 0.13 g, mp. 313°-315° C.

후처리

  1. extractionThe product was extracted into ethyl acetate
  2. dry with materialdried (MgSO4)
  3. customevaporated
  4. customThe residue was purified by chromatography on SiO2 gel
  5. washeluting with EtOAc to 8% MeOH/EtOAc

출처 및 근거

ORD 기록
ord-0201d33d717b481ca14ea4013d3e0e6a
출처 데이터셋
uspto-grants-1992_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05136080

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