Hydrazine hydrate (1:1) → 5-Bromo-2-hydrazinyl-3-methylpyridine

HRID 873992ノート

反応式

HRID 873992 の反応式
O.[NH2:2][NH2:3].[Br:4][C:5]1[CH:6]=[C:7]([CH3:12])[C:8](Cl)=[N:9][CH:10]=1>COCCO>[Br:4][C:5]1[CH:6]=[C:7]([CH3:12])[C:8]([NH:2][NH2:3])=[N:9][CH:10]=1

参加物

4

反応物 2

HCID 24654Hydrazine hydrate (1:1)HCID 2854345-Bromo-2-chloro-3-methylpyridine

生成物 1

HCID 534029825-Bromo-2-hydrazinyl-3-methylpyridine収率 49.1%

試薬・触媒・溶媒 1

HCID 80192-Methoxyethanol溶媒

反応条件

温度
120 °C

実験手順

Hydrazine hydrate (119 mL, 2422 mmol) was added to a suspension of 5-bromo-2-chloro-3-methylpyridine (50 g, 242 mmol) in 2-methoxyethanol (250 mL). The resulting solution was stirred 30 h at 120° C. and concentrated. The yellow residue was purified by trituration with H2O to provide the title compound (24 g) as a colorless solid. tR: 0.39 min (LC-MS 2); ESI-MS: 201.9 [M+H]+ (LC-MS 2)

後処理

  1. concentrationconcentrated
  2. customThe yellow residue was purified by trituration with H2O

出典と根拠

ORDレコード
ord-fda35ec996e743919d41ab1c27490192
出典データセット
uspto-grants-2015_03
特許番号
US08975417B2

反応ノート

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