Ammonia → 5-AMINO-6-CHLORO-2(TRIFLUOROMETHYL)-1H-IMIDAZO [4,5-b] PYRIDINE

HRID 437404ノート

反応式

HRID 437404 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]2[N:10](OC)[C:9]([C:13]([F:16])([F:15])[F:14])=[N:8][C:5]2=[N:6][CH:7]=1.[NH3:17]>CO>[NH2:17][C:7]1[N:6]=[C:5]2[N:8]=[C:9]([C:13]([F:16])([F:15])[F:14])[NH:10][C:4]2=[CH:3][C:2]=1[Cl:1]

参加物

4

反応物 2

HCID 222AmmoniaHCID 203599161-METHOXY-6-CHLORO-2-(TRIFLUOROMETHYL)-1H-IMIDAZO(4,5-b)PYRIDINE

生成物 1

HCID 537074975-AMINO-6-CHLORO-2(TRIFLUOROMETHYL)-1H-IMIDAZO [4,5-b] PYRIDINE

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

A 2.5 g. portion of 6-chloro-1-methoxy-2-(trifluoromethyl)-1-H-imidazo [4,5-b] pyridine was dissolved in 25 ml. of methanol, and the solution was saturated with gaseous ammonia. The reaction mixture was stirred at ambient temperature for 2 hours, and additional ammonia was periodically bubbled through the liquid phase. The solvent was then removed under vacuum, and the solid residue was taken up in ethyl ether and the solution was stirred with anhydrous magnesium sulfate and charcoal. The solids were then removed by filtration, and the filtrate was evaporated to dryness to yield about 2 g. of 5-amino-6-chloro-2-(trifluoromethyl)-1H-imidazo [4,5-b] pyridine, which was recrystallized from chloroform-methanol. The purified product melted at 241° -242° C. , and it was identified conclusively by infrared, nuclear magnetic resonance, mass spectroscopy and elemental microanalysis. The analytical results were as follows.

後処理

  1. customadditional ammonia was periodically bubbled through the liquid phase
  2. customThe solvent was then removed under vacuum
  3. stirringthe solution was stirred with anhydrous magnesium sulfate and charcoal
  4. customThe solids were then removed by filtration
  5. customthe filtrate was evaporated to dryness
  6. customto yield about 2 g
  7. customof 5-amino-6-chloro-2-(trifluoromethyl)-1H-imidazo [4,5-b] pyridine, which was recrystallized from chloroform-methanol
  8. customThe analytical results

出典と根拠

ORDレコード
ord-3e2365c1ddb149788188ec2e3e5d7051
出典データセット
uspto-grants-1977_06
特許番号
US04031107

反応ノート

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