Bromine → 2-Amino-3-bromo-5-methylpyrazine

HRID 361413

反応式

HRID 361413 の反応式
[Br:1]Br.[NH2:3][C:4]1[CH:9]=[N:8][C:7]([CH3:10])=[CH:6][N:5]=1>C(Cl)(Cl)Cl>[NH2:3][C:4]1[C:9]([Br:1])=[N:8][C:7]([CH3:10])=[CH:6][N:5]=1

参加物

4

反応物 2

HCID 24408BromineHCID 3132155-Methylpyrazin-2-amine

生成物 1

HCID 98990432-Amino-3-bromo-5-methylpyrazine

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒2 回

実験手順

A solution of bromine (0.11 ml) in chloroform (20 ml) was added dropwise over 20 minutes to a solution of 2-amino-5-methylpyrazine (0.218 g) in chloroform (30 ml) which was protected from light. The reaction mixture was stirred for 90 minutes after addition was complete and was then washed with water (50 ml). The organic phase was dried (MgSO4) and volatile material was removed by evaporation to give a yellow oil. The oil was purified by elution with dichloromethane through a silica gel Mega Bond Elut column to give 2-amino-3-bromo-5-methylpyrazine (0.286 g) as a white solid, m.p. 51°-52° C.; mass spectrum (+ve CI): 188 (M+H)+.

後処理

  1. additionafter addition
  2. washwas then washed with water (50 ml)
  3. dry with materialThe organic phase was dried (MgSO4) and volatile material
  4. customwas removed by evaporation
  5. customto give a yellow oil
  6. customThe oil was purified by elution with dichloromethane through a silica gel Mega Bond Elut column

出典と根拠

ORDレコード
ord-13e1cd739e3b4ec59ea400f3adfb8c5f
出典データセット
uspto-grants-1999_02
特許番号
US05866568

関連ノート

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