Sodium Carbonate → HCID 89462835、化合物

HRID 1525216ノート

反応式

HRID 1525216 の反応式
[Br:1][C:2]1[N:7]=[CH:6][C:5]([C:8]([C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=2)=O)=[CH:4][CH:3]=1.Cl.[OH:17][NH2:18].C(=O)([O-])[O-].[Na+].[Na+]>C(O)C>[Br:1][C:2]1[N:7]=[CH:6][C:5]([C:8]([C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=2)=[N:18][OH:17])=[CH:4][CH:3]=1

参加物

5

反応物 3

HCID 10340Sodium CarbonateHCID 443297Hydroxyamine hydrochlorideHCID 20145702(6-Bromopyridin-3-yl)(phenyl)methanone2 回

生成物 1

HCID 89462835HCID 89462835、化合物収率 50%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A solution of (6-bromopyridin-3-yl)(phenyl)methanone, 4-b, (5.2 g, 20 mmol) in 100 ml of 95% ethanol was treated with N-hydroxylamine hydrochloride (4.2 g, 60 mmol) and sodium carbonate (6.36 g, 60 mmol). The resulting mixture was heated at reflux for 3 hours, cooled to room temperature, and concentrated under vacuum. The residue was taken into ethyl acetate (100 mL) followed by washing with water and brine (50 mL each). The organic layer was dried over sodium sulfate and concentrated. The resulting solid was recrystallized in ethyl acetate/petroleum ether to provide the product, 4-c, (2.7 g, 50%). 1H NMR (CD3OD, 300 MHz,): δ 8.34 (s, 1H), 7.78 (m, 1H), 7.32 (m, 7H).

後処理

  1. temperatureThe resulting mixture was heated
  2. temperatureat reflux for 3 hours
  3. concentrationconcentrated under vacuum
  4. washby washing with water and brine (50 mL each)
  5. dry with materialThe organic layer was dried over sodium sulfate
  6. concentrationconcentrated
  7. customThe resulting solid was recrystallized in ethyl acetate/petroleum ether

出典と根拠

ORDレコード
ord-9d12023385564e5c8f2ffb6e29538e80
出典データセット
uspto-grants-2015_07
特許番号
US09079930B2

反応ノート

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