Hydrazine hydrate (1:1) → 6-(4-Fluorophenyl)-3-hydrazinyl-1,2,4-triazine

HRID 1099034ノート

反応式

HRID 1099034 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][C:14]([F:17])=[CH:13][CH:12]=2)=[CH:9][N:10]=1>N1C=CC=CC=1>[F:17][C:14]1[CH:15]=[CH:16][C:11]([C:8]2[N:7]=[N:6][C:5]([NH:2][NH2:3])=[N:10][CH:9]=2)=[CH:12][CH:13]=1

参加物

4

反応物 2

HCID 24654Hydrazine hydrate (1:1)HCID 213152193-Chloro-6-(4-fluorophenyl)-1,2,4-triazine

生成物 1

HCID 213152186-(4-Fluorophenyl)-3-hydrazinyl-1,2,4-triazine収率 91.9%

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 (0.28 mL, 0.0057 mol) was added to a suspension of 3-chloro-6-(4-fluorophenyl)-1,2,4-triazine (400 mg, 0.002 mol) in pyridine (4 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 solid was collected and dried under high vacuum to give the desired product (360 mg, 91.9%). Analytical LCMS: (M+H)+=206.1.

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 solid was collected
  8. customdried under high vacuum

出典と根拠

ORDレコード
ord-9108564c25fe4982a19aeebc9494f256
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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