Phosphorus oxychloride → 4-Chloro-6-methyl-5-propylpyrimidine
反応式
[CH2:1]([C:4]1[C:5](=O)[NH:6][CH:7]=[N:8][C:9]=1[CH3:10])[CH2:2][CH3:3].O=P(Cl)(Cl)[Cl:14]>>[CH2:1]([C:4]1[C:5]([Cl:14])=[N:6][CH:7]=[N:8][C:9]=1[CH3:10])[CH2:2][CH3:3]参加物
3
反応条件
- 温度
- 85 °C
実験手順
A mixture of 5-propyl-6-methyl-pyrimidin4-one (10 mmol) and POCl3 (25 ml) is heated at 85° C. for 4 hours. The solvent is removed in vacuo and EtOAc (30 ml) and water (30 ml) are added to the residue. NaHCO3 is carefully added until the pH of aqueous layer is greater than 7. The layers are separated and the aqueous layer is extracted with EtOAc (2×30 ml). The combined extracts are washed with brine (50 ml), dried (Na2SO4), and evaporated. Flash column purification of the residue with 6:1 EtOAc:hexane provides the title product as a light yellow oil.
後処理
- customThe solvent is removed in vacuo and EtOAc (30 ml) and water (30 ml)
- additionare added to the residue
- additionNaHCO3 is carefully added until the pH of aqueous layer
- customThe layers are separated
- extractionthe aqueous layer is extracted with EtOAc (2×30 ml)
- washThe combined extracts are washed with brine (50 ml)
- dry with materialdried (Na2SO4)
- customevaporated
- customFlash column purification of the residue with 6:1 EtOAc
出典と根拠
- ORDレコード
- ord-fa43245339f34a73975084265eff21d7
- 出典データセット
- uspto-grants-2008_04
- 特許番号
- US07351826B2
反応ノート
読み込み中…