Water → Methyl 4-bromo-3-methoxythiophene-2-carboxylate
反応式
[Br:1][C:2]1[C:3]([OH:11])=[C:4]([C:7]([O:9][CH3:10])=[O:8])[S:5][CH:6]=1.CI.[C:14]([O-])([O-])=O.[K+].[K+].O>CS(C)=O>[Br:1][C:2]1[C:3]([O:11][CH3:14])=[C:4]([C:7]([O:9][CH3:10])=[O:8])[S:5][CH:6]=1参加物
6
実験手順
To a solution of 36 g (0.15 mole) of methyl 4-bromo-3-hydroxy-2-thiophenecarboxylate in 300 mL of dimethyl sulfoxide (DMSO) was added 32 g (0.23 mole) of methyl iodide and then 32 g of powdered K2CO3. After 2 hr, the reaction mixture was poured into water and extracted with ether. The organic phase was washed with water (4×200 mL), dried over MgSO4, filtered and concentrated to give 36 g of a colorless solid. 1H NMR (300 MHz, CDCl3): δ 7.4 (s, 1H); 4.0 (s, 3H); 3.9 (s, 3H). Anal. Calc'd for C7H7BrO3S: C, 33.48; H, 2.81; S, 12.77. Found: C, 33.18; H, 2.70; S, 12.49.
後処理
- extractionextracted with ether
- washThe organic phase was washed with water (4×200 mL)
- dry with materialdried over MgSO4
- filtrationfiltered
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-8cbb7dfa86b3486483d3ea847e70e751
- 出典データセット
- uspto-grants-2003_11
- 特許番号
- US06645918B1
反応ノート
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