三氯氧磷 → 4-Chloro-6-methyl-5-propylpyrimidine
反应方程式
[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]参与物
3
反应条件
- 温度
- 85 °C
实验过程
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.
后处理
- 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
来源与证据
- ORD记录
- ord-fa43245339f34a73975084265eff21d7
- 来源数据集
- uspto-grants-2008_04
- 专利号
- US07351826B2
反应笔记
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