HRID78745

反应详情

EQUATION

反应方程式

HRID 78745 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
-2.5 °C

PROCEDURE

实验过程

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).

WORKUP

后处理

  1. temperatureby maintaining temp below 0° C
  2. customReaction mass
  3. customReaction mass
  4. concentrationwas concentrated to residue under vacuum at 40° C
  5. dissolutionResidue was dissolved in Ethyl acetate (450 ml)
  6. washwashed with sodium sulphite solution (10%, 2×135 ml)
  7. customReaction mass
  8. concentrationwas then concentrated to residue