HCID 15580721、化合物 → HCID 15580712、化合物
反応式
[Cl:1][C:2]1[CH:3]=[C:4]([N:9]2[CH2:13][CH:12]([CH3:14])[C:11]([NH:15][CH:16]=[O:17])=[N:10]2)[CH:5]=[CH:6][C:7]=1Cl>C(O)=O>[Cl:1][C:2]1[CH:3]=[C:4]([N:9]2[CH2:13][CH:12]([CH3:14])[C:11]([NH:15][CH:16]=[O:17])=[N:10]2)[CH:5]=[CH:6][CH:7]=1参加物
3
実験手順
A 3.0 g. amount of the preceding product is dissolved in 10 ml. of a mixture of formic acid and acetic anhydride (Example 15). The mixture is allowed to remain at room temperature for 3 hours, then is poured into ice water to separate a partial gum and solid. This material is collected, dissolved in dichloromethane and filtered through a short column of a hydrous magnesium silicate. The effluent is concentrated while adding hexane to separate 3.1 g. of the product of the Example as light yellow crystals, m.p. 140°-142° C.
後処理
- dissolutionamount of the preceding product is dissolved in 10 ml
- customto separate a partial gum and solid
- customThis material is collected
- dissolutiondissolved in dichloromethane
- filtrationfiltered through a short column of a hydrous magnesium silicate
- concentrationThe effluent is concentrated
- additionwhile adding hexane
- customto separate 3.1 g
出典と根拠
- ORDレコード
- ord-3e0339da476046bbb3ec83612c760475
- 出典データセット
- uspto-grants-1982_09
- 特許番号
- US04348527
反応ノート
読み込み中…