6-chloro-N4-o-tolylpyrimidine-4,5-diamine → HCID 57438664、化合物

HRID 1098226ノート

反応式

HRID 1098226 の反応式
[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

参加物

5

反応物 2

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

生成物 1

HCID 57438664HCID 57438664、化合物収率 94%

試薬・触媒・溶媒 2

HCID 176Acetic Acid溶媒HCID 6344Dichloromethane溶媒

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-0ef68f50d3a0490db7537973997e3a39
出典データセット
uspto-grants-2012_03
特許番号
US08143263B2

反応ノート

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