Sodium Carbonate → HCID 89462835, 화합물

HRID 1525216노트

반응식

HRID 1525216 반응식
[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

참가 물질

5

반응물 3

HCID 10340Sodium CarbonateHCID 443297Hydroxyamine hydrochlorideHCID 20145702(6-Bromopyridin-3-yl)(phenyl)methanone2회

생성물 1

HCID 89462835HCID 89462835, 화합물수율 50%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-9d12023385564e5c8f2ffb6e29538e80
출처 데이터셋
uspto-grants-2015_07
특허 번호
US09079930B2

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