Triethylamine → HCID 22139808、化合物
反応式
[C:1]([NH:4][C:5]1[C:9]([Cl:10])=[C:8](Cl)[S:7][C:6]=1[C:12]([O:14][CH3:15])=[O:13])(=[O:3])[CH3:2].C(N(CC)CC)C.[H][H]>[Pd].CO>[C:1]([NH:4][C:5]1[C:9]([Cl:10])=[CH:8][S:7][C:6]=1[C:12]([O:14][CH3:15])=[O:13])(=[O:3])[CH3:2]参加物
6
実験手順
A mixture of 25 g of methyl 3-acetylamino-4,5-dichlorothiophene-2-carboxylate, about 10 g of triethylamine, 300 ml of methanol and 1 g of palladium on carbon is, at room temperature and under atmospheric pressure, hydrogenated until the uptake of hydrogen has stopped. The catalyst is filtered off and the mixture is then concentrated by distillation under reduced pressure until crystallization begins, water is then added and the solid is filtered off. Colorless crystals from isopropanol. M.p. 142-147° C.
後処理
- customis, at room temperature and under atmospheric pressure
- filtrationThe catalyst is filtered off
- concentrationthe mixture is then concentrated by distillation under reduced pressure until crystallization
- additionwater is then added
- filtrationthe solid is filtered off
出典と根拠
- ORDレコード
- ord-865ae88bdb254a7886a2e23f40c0be52
- 出典データセット
- uspto-grants-2006_05
- 特許番号
- US07049333B2
反応ノート
読み込み中…