HRID1259403

反应详情

EQUATION

反应方程式

HRID 1259403 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Borane-DMS (0.2 mL, 2.3 mmol) was added to a solution of diethyl 2-(3-(butoxysulfonyl)cyclobutylidene)malonate (0.2 g, 0.575 mmol) in THF (5 mL) and the resulting reaction mass was stirred at room temperature overnight. The reaction was monitored by TLC (100% ethyl acetate). The reaction mixture was quenched with 1N HCl and extracted using ethyl acetate. The organic layer was washed with brine solution, dried over anhydrous Na2SO4 and concentrated. Purification by column chromatography on silica gel (70% ethyl acetate in hexane) afforded 0.13 g of the product (74% yield).

WORKUP

后处理

  1. customthe resulting reaction mass
  2. customThe reaction mixture was quenched with 1N HCl
  3. extractionextracted
  4. washThe organic layer was washed with brine solution
  5. dry with materialdried over anhydrous Na2SO4
  6. concentrationconcentrated
  7. customPurification by column chromatography on silica gel (70% ethyl acetate in hexane)