反応 #165927

反応方程式

Ethyl-2-(4,5-dihydrofuran-3-yl)-2-oxoacetate

tetrahydrofuran

N-bromosuccinimide

→

ethyl-2-(3-bromo-2-methoxytetrahydrofuran-3-yl)-2-oxoacetate

溶媒

Methanol

反応条件

後処理

1. 1
   温度by maintaining temp below 0° C
2. 2
   その他Reaction mass
3. 3
   その他Reaction mass
4. 4
   濃縮was concentrated to residue under vacuum at 40° C
5. 5
   workup.DISSOLUTIONResidue was dissolved in Ethyl acetate (450 ml)
6. 6
   洗浄washed with sodium sulphite solution (10%, 2×135 ml)
7. 7
   その他Reaction mass
8. 8
   濃縮was then concentrated to residue

実験手順

Ethyl-2-(4,5-dihydrofuran-3-yl)-2-oxoacetate (45 g) was dissolved in tetrahydrofuran (225 ml) and Methanol (45 ml). The reaction mass was cooled to −5 to 0° C. N-bromosuccinimide (47 g) was added lot wise by maintaining temp below 0° C. Reaction mass was then stirred at 20-25° C. for 12 hrs. Reaction mass was concentrated to residue under vacuum at 40° C. Residue was dissolved in Ethyl acetate (450 ml) and washed with sodium sulphite solution (10%, 2×135 ml). Reaction mass was then concentrated to residue to get ethyl-2-(3-bromo-2-methoxytetrahydrofuran-3-yl)-2-oxoacetate (Yield 63 g).

出典