Bromine → 4-Bromo-6-phenylpyridazin-3-amine

HRID 1755307ノート

反応式

HRID 1755307 の反応式
[C:1]1([C:7]2[N:12]=[N:11][C:10]([NH2:13])=[CH:9][CH:8]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.C([O-])(O)=O.[Na+].[Br:19]Br>CO>[Br:19][C:9]1[CH:8]=[C:7]([C:1]2[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=2)[N:12]=[N:11][C:10]=1[NH2:13]

参加物

5

反応物 3

HCID 24408BromineHCID 516892Sodium BicarbonateHCID 119589156-Phenylpyridazin-3-amine

生成物 1

HCID 583863604-Bromo-6-phenylpyridazin-3-amine収率 33.1%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

In a 150 mL round bottom flask was placed 6-phenylpyridazin-3-amine (2.5 g, 14.5 mmol), NaHCO3 (2.44 g, 29 mmol) and methanol (50 mL) then to this suspension was added Br2 (2.317 g, 14.5 mmol) drop wise over about 30 minutes at room temperature. The mixture was stirred for 16 h, then filtered and concentrated in vacuo. The residue was purified by chromatography (silica gel, 200-300 mesh, petroleum ether:ethyl acetate=2:1) to give 4-bromo-6-phenylpyridazin-3-amine (1.2 g, 33%) as a light orange solid. LC-MS: [M+H]+, 250.0, tR=1.487 min.

後処理

  1. customIn a 150 mL round bottom flask was placed
  2. filtrationfiltered
  3. concentrationconcentrated in vacuo
  4. customThe residue was purified by chromatography (silica gel, 200-300 mesh, petroleum ether:ethyl acetate=2:1)

出典と根拠

ORDレコード
ord-dc69f5c8911d47afb49c0a67735122db
出典データセット
uspto-grants-2015_10
特許番号
US09169259B2

反応ノート

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