Dimethyl Sulfide → (2-Ethoxy-2-oxoethyl)dimethylsulphonium bromide
반응식
[Br:1][CH2:2][C:3]([O:5][CH2:6][CH3:7])=[O:4].[CH3:8][S:9][CH3:10]>CC(C)=O>[Br-:1].[CH2:6]([O:5][C:3]([CH2:2][S+:9]([CH3:10])[CH3:8])=[O:4])[CH3:7]참가 물질
4
실험 절차
A stirred solution of ethyl bromoacetate (98%, 287 g, 1.68 mol) and methyl sulfide (99%, 156 mL, 1.25 eq.) in acetone (500 mL) was kept at 15° C. A white precipitate started to appear immediately and became thicker upon stirring. After stirring for 18 h at 22° C., the solid was filtered, washed with acetone (3×100 mL), and dried under vacuum to afford 1 (477 g, 83.4%) as white crystals. 1H NMR (250 MHz, CDCl3) δ 5.20 (s, 2H); 4.29 (q, J=7.2, 2H); 3.46 (s, 6H); 1.32 (t, J=7.2, 3H). 13C NMR (62.5 MHz, CDCl3) δ 164.36; 63.38; 44.38; 25.22; 13.92.
후처리
- customwas kept at 15° C
- stirringAfter stirring for 18 h at 22° C.
- filtrationthe solid was filtered
- washwashed with acetone (3×100 mL)
- customdried under vacuum
출처 및 근거
- ORD 기록
- ord-09a9dbf030b6474c95c16db7d2a41a03
- 출처 데이터셋
- uspto-grants-2008_11
- 특허 번호
- US07453011B2
반응 노트
불러오는 중…