6-chloro-N4-o-tolylpyrimidine-4,5-diamine → HCID 57438664, 화합물

HRID 1098226노트

반응식

HRID 1098226 반응식
[N:1]([O-])=O.[Na+].[Cl:5][C:6]1[N:11]=[CH:10][N:9]=[C:8]([NH:12][C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][C:14]=2[CH3:19])[C:7]=1[NH2:20]>C(O)(=O)C.C(Cl)Cl>[Cl:5][C:6]1[C:7]2[N:20]=[N:1][N:12]([C:13]3[CH:18]=[CH:17][CH:16]=[CH:15][C:14]=3[CH3:19])[C:8]=2[N:9]=[CH:10][N:11]=1

참가 물질

5

반응물 2

HCID 234775416-chloro-N4-o-tolylpyrimidine-4,5-diamineHCID 23668193Sodium Nitrite

생성물 1

HCID 57438664HCID 57438664, 화합물수율 94%

시약·촉매·용매 2

HCID 176Acetic Acid용매HCID 6344Dichloromethane용매

실험 절차

Sodium nitrite (0.323 g, 4.69 mmol) was added to 6-chloro-N4-o-tolylpyrimidine-4,5-diamine (Intermediate AP5)(1 g, 4.26 mmol) in acetic acid (50% Aq) (25 mL)and DCM (25 mL) at room temperature. The resulting solution was stirred at room temperature for 15 minutes. The reaction mixture was separated and the organic phase was washed with water (10 mL), dried (MgSO4) and evaporated to give crude 7-chloro-3-o-tolyl-3H-[1,2,3]triazolo[4,5-d]pyrimidine (0.980 g, 94%) that was used without further purification.

후처리

  1. customThe reaction mixture was separated
  2. washthe organic phase was washed with water (10 mL)
  3. dry with materialdried (MgSO4)
  4. customevaporated

출처 및 근거

ORD 기록
ord-0ef68f50d3a0490db7537973997e3a39
출처 데이터셋
uspto-grants-2012_03
특허 번호
US08143263B2

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