Water → 6-Chloro-3-hydrazinyl-4-methylpyridazine

HRID 874013

反応式

HRID 874013 の反応式
Cl[C:2]1[N:3]=[N:4][C:5]([Cl:9])=[CH:6][C:7]=1[CH3:8].O.[NH2:11][NH2:12].O>CCO>[Cl:9][C:5]1[N:4]=[N:3][C:2]([NH:11][NH2:12])=[C:7]([CH3:8])[CH:6]=1

参加物

5

反応物 3

HCID 962WaterHCID 24654Hydrazine hydrate (1:1)HCID 879233,6-Dichloro-4-methylpyridazine

生成物 1

HCID 114464906-Chloro-3-hydrazinyl-4-methylpyridazine収率 39.1%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
80 °C

実験手順

3,6-Dichloro-4-methylpyridazine (Combi-Blocks) (60 g, 361 mmol) was dissolved in hydrazine monohydrate (Aldrich) (335 mL, 5411 mmol) and the solution was stirred at 80° C. for 1 h, forming a white precipitate. The reaction mixture is dilutes with water and the precipitated products isolated by filtration. The solid crude product is suspended in EtOH and left in an ultra sound bath for 1 h. The desired product (22.4 g) was obtained after filtration and drying under vacuum as a beige solid. tR: 0.31 min (LC-MS 2); ESI-MS: 160.0 [M+H]+ (LC-MS 2). 1H NMR (400 MHz; DMSO-d6) δ ppm 7.83 (br.s, 1H) 7.32 (s, 1H) 4.49 (br.s, 2H) 2.05 (s, 3H).

後処理

  1. customforming a white precipitate
  2. customthe precipitated products isolated by filtration
  3. waitleft in an ultra sound bath for 1 h

出典と根拠

ORDレコード
ord-cb3edca2b4dd4f3fab854d9cc4acc786
出典データセット
uspto-grants-2015_03
特許番号
US08975417B2

関連ノート

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