Triethylamine → 2-Bromo-N-(6-methyl-pyridazin-3-yl)-acetamide

HRID 2192376ノート

反応式

HRID 2192376 の反応式
[Br:1][CH2:2][C:3](Br)=[O:4].[NH2:6][C:7]1[N:8]=[N:9][C:10]([CH3:13])=[CH:11][CH:12]=1.C(N(CC)CC)C>C(Cl)(Cl)Cl>[Br:1][CH2:2][C:3]([NH:6][C:7]1[N:8]=[N:9][C:10]([CH3:13])=[CH:11][CH:12]=1)=[O:4]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 61147Bromoacetyl bromideHCID 877126-Methylpyridazin-3-amine

生成物 1

HCID 673108012-Bromo-N-(6-methyl-pyridazin-3-yl)-acetamide

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒2 回

実験手順

A solution of bromoacetyl bromide (0.22 mL) in dry CHCl3 (4 mL) was added slowly to a suspension of 3-amino-6-methylpyridazine (0.24 g) and triethylamine (0.47 mL) in dry CHCl3 (45 mL) at room temperature. The brown mixture was allowed to stir for 3.5 hr, then quenched with H2O (1.5 mL) and stirred for 20 mins before concentrating under reduced pressure to a brown solid. The crude product was purified by silica gel chromatography eluting with 1-2% MeOH/dichloromethane. The relevant fractions were combined and evaporated to give the title compound (0.20 g) as a pinkish/beige solid.

後処理

  1. customquenched with H2O (1.5 mL)
  2. stirringstirred for 20 mins
  3. concentrationbefore concentrating under reduced pressure to a brown solid
  4. customThe crude product was purified by silica gel chromatography
  5. washeluting with 1-2% MeOH/dichloromethane
  6. customevaporated

出典と根拠

ORDレコード
ord-f936bb35d18b4f92b12d235e0b7d0eff
出典データセット
uspto-grants-2012_12
特許番号
US08329729B2

反応ノート

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