反応 #1265380
ord-fbe8899a89ce4e0381341edcbacf41d6
反応方程式
n-BuLi
4-methylthiazole
N-methoxy-N-methylacetamide
→
2a
収率 85.0%
1-(4-Methyl-thiazol-2-yl)-ethanone
収率 85.0%
反応条件
詳細条件
See reaction.notes.procedure_details.
後処理
- 1workup.STIRRINGAfter 1 h of stirring at −78° C. the reaction mixture
- 2洗浄was washed with sat'd NaHCO3
- 3抽出extracted with ether
- 4乾燥The organic layer was dried with Na2SO4
- 5濃縮concentrated in vacuo
実験手順
To a stirred solution of n-BuLi (2M in pentane; 22.4 mL, 0.045 mol) in 70 mL of dry ether at −78° C. was added dropwise 4-methylthiazole (3.7 g, 0.037 mol) in 30 mL of ether over a period of 30 minutes. The mixture was stirred for 1 h, then N-methoxy-N-methylacetamide (4.37 mL, 0.041 mol) was added dropwise over 10 minutes. After 1 h of stirring at −78° C. the reaction mixture was washed with sat'd NaHCO3 and extracted with ether. The organic layer was dried with Na2SO4 and concentrated in vacuo to give 4.38 g (85%) of 2a as an oil that was used directly for the next step. 1H NMR (CDCl3) δ 7.2 (s, 1H), 2.75 (s, 3H), 2.5 (s, 3H).