Acetic Anhydride → (3-Methylthiophen-2-yl)methyl acetate
반응식
[CH3:1][C:2]1[CH:6]=[CH:5][S:4][C:3]=1[CH2:7][OH:8].[C:9](OC(=O)C)(=[O:11])[CH3:10]>N1C=CC=CC=1.CCOC(C)=O>[C:9]([O:8][CH2:7][C:3]1[S:4][CH:5]=[CH:6][C:2]=1[CH3:1])(=[O:11])[CH3:10]참가 물질
5
실험 절차
To a solution of 62.2 (0.87 g, 6.79 mmol) in pyridine (20 mL) was added acetic anhydride (0.8 mL, 8.14 mmol) at room temperature. The mixture was stirred overnight at room temperature, diluted with EtOAc, washed with 1N HCl and brine, dried (Na2SO4), and concentrated. The crude product was chromatographed on silica gel (0-15% EtOAc/hexane) to afford 62.3. 1H NMR (400 MHz, CDCl3) δ 7.21 (d, 1H), 6.84 (d, 1H), 5.20 (s, 2H), 2.26 (s, 3H), 2.08 (s, 3H).
후처리
- washwashed with 1N HCl and brine
- dry with materialdried (Na2SO4)
- concentrationconcentrated
- customThe crude product was chromatographed on silica gel (0-15% EtOAc/hexane)
출처 및 근거
- ORD 기록
- ord-21810cb283e145759eb80ec1e59c99ea
- 출처 데이터셋
- uspto-grants-2011_08
- 특허 번호
- US08003648B2
반응 노트
불러오는 중…