Phosphorus oxychloride → Ethyl-2-methoxymethyl-4-chloropyrimidine-5-acetate
反応式
[CH3:1][O:2][CH2:3][C:4]1[N:9]=[C:8](O)[C:7]([CH2:11][C:12]([O:14][CH2:15][CH3:16])=[O:13])=[CH:6][N:5]=1.P(Cl)(Cl)([Cl:19])=O>>[CH2:15]([O:14][C:12](=[O:13])[CH2:11][C:7]1[C:8]([Cl:19])=[N:9][C:4]([CH2:3][O:2][CH3:1])=[N:5][CH:6]=1)[CH3:16]参加物
3
実験手順
A mixture of the product of Step 1, above (0.01 mol) and phosphorous oxychloride (7 ml) was refluxed for 20 minutes. The excess phosphorous oxychloride was removed, the residue was quenched with ice water (15 ml) and the mixture was extracted with ethyl acetate (2×20 ml). The ethyl acetate layer was collected and washed with water (2×10 ml). The organic extract was collected, dried over MgSO4 and the dried portion was evaporated to obtain the title compound as an oil (78% yield).
後処理
- customThe excess phosphorous oxychloride was removed
- customthe residue was quenched with ice water (15 ml)
- extractionthe mixture was extracted with ethyl acetate (2×20 ml)
- customThe ethyl acetate layer was collected
- washwashed with water (2×10 ml)
- extractionThe organic extract
- customwas collected
- dry with materialdried over MgSO4
- customthe dried portion was evaporated
出典と根拠
- ORDレコード
- ord-7d69c9c0cd244e8aa1776baa6ae8f9ea
- 出典データセット
- uspto-grants-1998_08
- 特許番号
- US05789415
反応ノート
読み込み中…