Hydrazine hydrate (1:1) → 3-Amino-6-bromopyrazine-2-carbohydrazide

HRID 78726

反応式

HRID 78726 の反応式
[NH2:1][C:2]1[C:3]([C:9]([O:11]C)=O)=[N:4][C:5]([Br:8])=[CH:6][N:7]=1.O.[NH2:14][NH2:15]>O1CCOCC1>[NH2:1][C:2]1[C:3]([C:9]([NH:14][NH2:15])=[O:11])=[N:4][C:5]([Br:8])=[CH:6][N:7]=1

参加物

4

反応物 2

HCID 24654Hydrazine hydrate (1:1)HCID 227251Methyl 3-Amino-6-bromopyrazine-2-carboxylate

生成物 1

HCID 580702563-Amino-6-bromopyrazine-2-carbohydrazide

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

反応条件

温度
60 °C

実験手順

Methyl 3-amino-6-bromopyrazine-2-carboxylate (15 g, 64.6 mmol) was suspended in 150 mL of dioxane at room temperature. Hydrazine hydrate (6.5 g, 130 mmol) was added and the reaction mixture was stirred at 60° C. for 2 hours. Initially the mixture became clear, but after a while a precipitate formed. The mixture was cooled to ambient temperature and crude product filtered off. The solid was washed with TBME and subsequently stirred in water. The material was filtered and washed with acetone to afford 3-Amino-6-bromopyrazine-2-carbohydrazide 4 as slightly yellow solid. The material was dried in vacuo. (10.5 g, 70%).

後処理

  1. customafter a while a precipitate formed
  2. temperatureThe mixture was cooled to ambient temperature
  3. filtrationcrude product filtered off
  4. washThe solid was washed with TBME
  5. stirringsubsequently stirred in water
  6. filtrationThe material was filtered
  7. washwashed with acetone

出典と根拠

ORDレコード
ord-be4ae37bcf25498c950d1b45beb2a192
出典データセット
uspto-grants-2014_09
特許番号
US08841449B2

関連ノート

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