Hydrazine hydrate (1:1) → 3-Hydrazino-6-phenyl-1,2,4-triazine

HRID 1099032ノート

反応式

HRID 1099032 の反応式
O.[NH2:2][NH2:3].Cl[C:5]1[N:6]=[N:7][C:8]([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)=[CH:9][N:10]=1>N1C=CC=CC=1>[NH:2]([C:5]1[N:6]=[N:7][C:8]([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)=[CH:9][N:10]=1)[NH2:3]

参加物

4

反応物 2

HCID 24654Hydrazine hydrate (1:1)HCID 110306323-Chloro-6-phenyl-1,2,4-triazine

生成物 1

HCID 64051603-Hydrazino-6-phenyl-1,2,4-triazine収率 93%

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

反応条件

温度
0 °C

実験手順

Hydrazine hydrate (1.50 mL, 0.0308 mol) was added to suspension of 3-chloro-6-phenyl-1,2,4-triazine (2.20 g, 0.0115 mol) in pyridine (12.0 mL) at 0° C. and stirred at 0° C. until a precipitate formed. The mixture was then heated at 65° C. for 30 min. The solvent was evaporated under reduced pressure. The residue was triturated with water, filtered, and washed with water. The crystalline formed was collected and dried under high vacuum to give the desired product (2.0 g, 93%). Analytical LCMS: (M+H)+=188.1.

後処理

  1. customformed
  2. temperatureThe mixture was then heated at 65° C. for 30 min
  3. customThe solvent was evaporated under reduced pressure
  4. customThe residue was triturated with water
  5. filtrationfiltered
  6. washwashed with water
  7. customThe crystalline formed
  8. customwas collected
  9. customdried under high vacuum

出典と根拠

ORDレコード
ord-1fe9dd1f9bb44cd9b77e5baa16aa9e03
出典データセット
uspto-grants-2012_03
特許番号
US08143251B2

反応ノート

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