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Potassium Carbonate → 5-Bromo-N,N-dimethylpyridin-3-amine

HRID 589451
ノート
印刷プレビュー

反応式

HRID 589451 の反応式
[Br:1][C:2]1[CH:3]=[N:4][CH:5]=[C:6](Br)[CH:7]=1.C([O-])([O-])=O.[K+].[K+].[CH3:15][N:16](Cl)[CH3:17]>CN(C=O)C>[Br:1][C:2]1[CH:7]=[C:6]([N:16]([CH3:17])[CH3:15])[CH:5]=[N:4][CH:3]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 693693,5-DibromopyridineHCID 123122N-Chlorodimethylamine

生成物 1

HCID 234368635-Bromo-N,N-dimethylpyridin-3-amine収率 88.5%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
200 °C

実験手順

To a solution of 3,5-dibromopyridine (XLII) (2.37 g, 10.0 mmol) in dry DMF (20.0 mL) was added K2CO3 (4.5 g, 33 mmol) and dimethylamino hydrochloride (1.79 g, 22 mmol). The mixture was heated overnight at 200° C. in a sealed tube. The solution was cooled to room temperature and excess DMF was removed under vacuum. The residue was partitioned between EtOAc and water. The organic phase was separated. The aqueous phase was washed with EtOAc and the combined organic phases were dried over MgSO4, and concentrated to afford 5-bromo-N,N-dimethylpyridin-3-amine (XLIII) as an off-white solid (1.78 g, 8.85 mmol, 88% yield). 1H NMR (DMSO-d6, 500 MHz) δ ppm 2.94 (s, 6H), 7.25 (t, J=2 Hz, 1H), 7.91 (d, J=2 Hz, 1H), 8.07 (d, J=2 Hz, 1H); ESIMS found C7H9BrN2 m/z 201.1 (M+H).

後処理

  1. temperatureThe solution was cooled to room temperature
  2. customexcess DMF was removed under vacuum
  3. customThe residue was partitioned between EtOAc and water
  4. customThe organic phase was separated
  5. washThe aqueous phase was washed with EtOAc
  6. dry with materialthe combined organic phases were dried over MgSO4
  7. concentrationconcentrated

出典と根拠

ORDレコード
ord-11801f2dd52a48ea83dfb83ac8c7f874
出典データセット
uspto-grants-2016_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09233104B2

反応ノート

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