Carbamide Peroxide → 3-Bromo-6-ethoxy-2-methoxypyridine
反応式
[Br:1][C:2]1[CH:3]=[CH:4][C:5]([O:8][CH2:9][CH3:10])=[N:6][CH:7]=1.OO.N[C:14](N)=[O:15]>C(Cl)Cl>[Br:1][C:2]1[C:7]([O:15][CH3:14])=[N:6][C:5]([O:8][CH2:9][CH3:10])=[CH:4][CH:3]=1参加物
4
実験手順
To 5.00 g (24.7 mmol) 5-bromo-2-ethoxy-pyridine in 50 mL DCM are added 4.66 g (49.5 mmol) urea hydrogen peroxide. Then the mixture is chilled to 0° C. before 6.88 mL (49.5 mmol) TFA anhydride are added. Afterwards cooling is removed and the resulting mixture is stirred over night while the temperature raises to r.t. The solvent is removed in vacuo, water is added and the resulting mixture is extracted with DCM. The combined org. layers are dried over MgSO4, filtered and the sovent is removed in vacuo. The crude product is purified by column chromatography (silica gel, DCM/MeOH).
後処理
- additionare added
- temperatureAfterwards cooling
- customis removed
- customThe solvent is removed in vacuo, water
- additionis added
- extractionthe resulting mixture is extracted with DCM
- dry with materiallayers are dried over MgSO4
- filtrationfiltered
- customthe sovent is removed in vacuo
- customThe crude product is purified by column chromatography (silica gel, DCM/MeOH)
出典と根拠
- ORDレコード
- ord-ca4c1f1787f5427985a3234ebe7520ed
- 出典データセット
- uspto-grants-2014_11
- 特許番号
- US08877741B2
反応ノート
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