Acetic Anhydride → 4-Acetamidothiazole
반응식
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]1참가 물질
6
실험 절차
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%).
후처리
- 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)
출처 및 근거
- ORD 기록
- ord-378b4c25c35a4c78ab8253f496edd2e5
- 출처 데이터셋
- uspto-grants-2016_07
- 특허 번호
- US09388180B2
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