Acetic Anhydride → 4-Acetamidothiazole
反応式
C(O[C:5](=[O:7])[CH3:6])(=O)C.Cl.[S:9]1[CH:13]=[C:12]([NH2:14])[N:11]=[CH:10]1.C(N(CC)CC)C>C(Cl)Cl.O>[S:9]1[CH:13]=[C:12]([NH:14][C:5](=[O:7])[CH3:6])[N:11]=[CH:10]1参加物
6
実験手順
Acetic anhydride (153 mg, 1.50 mmol) was added to the solution of thiazol-4-amine hydrochloride from example 2.2 (100 mg, 1.0 mmol) and triethylamine (152 mg, 1.50 mmol) in DCM (5 mL). The solution was stirred for overnight at room temperature. The reaction mixture was diluted with water, washed with 0.1 M HCl (10 mL), NaHCO3 solution and brine. The combined organic layers were dried with Na2SO4, filtered and concentrated. The resulting mixture was deposited onto silica gel and loaded onto a silica gel column and eluted with EA/PE (1:2) to aim product (55 mg, 0.39 mmol, 38.7%).
後処理
- washwashed with 0.1 M HCl (10 mL), NaHCO3 solution and brine
- dry with materialThe combined organic layers were dried with Na2SO4
- filtrationfiltered
- concentrationconcentrated
- washeluted with EA/PE (1:2)
出典と根拠
- ORDレコード
- ord-378b4c25c35a4c78ab8253f496edd2e5
- 出典データセット
- uspto-grants-2016_07
- 特許番号
- US09388180B2
反応ノート
読み込み中…