HCID 824395、化合物 → HCID 19349977、化合物
反応式
[C:1]([NH:4][NH:5][C:6](=[O:14])[C:7]1[CH:12]=[CH:11][CH:10]=[C:9]([I:13])[CH:8]=1)(=O)[CH3:2]>O=P(Cl)(Cl)Cl>[I:13][C:9]1[CH:8]=[C:7]([C:6]2[O:14][C:1]([CH3:2])=[N:4][N:5]=2)[CH:12]=[CH:11][CH:10]=1参加物
3
実験手順
The product obtained in Step A above (2.9 g, 9.54 mmol) is heated at 120° C. for 3 hours in 35 ml of POCl3. After evaporation of POCl3, the residue is taken up in toluene and the mixture is evaporated to dryness again. The residue from evaporation is dissolved in ethyl acetate and the organic phase is washed with, in succession, 10% NaHCO3 solution, water and then brine. The organic phase is dried over MgSO4 to yield, after evaporation, the expected product in the form of a creamy white solid.
後処理
- customAfter evaporation of POCl3
- customthe mixture is evaporated to dryness again
- customThe residue from evaporation
- dissolutionis dissolved in ethyl acetate
- washthe organic phase is washed with, in succession, 10% NaHCO3 solution, water
- dry with materialThe organic phase is dried over MgSO4
- customto yield
- customafter evaporation
出典と根拠
- ORDレコード
- ord-04d462ce02bc451a82f8f65efa7e4724
- 出典データセット
- uspto-grants-2013_10
- 特許番号
- US08569285B2
反応ノート
読み込み中…