HRID1257438

反应详情

EQUATION

反应方程式

HRID 1257438 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution (4 mL) of the compound (0.80 g) obtained in Example 128c in tetrahydrofuran was cooled in an ice bath, and lithium aluminum hydride (0.16 g) was added by small portions. The reaction mixture was stirred at the same temperature for 1 hr, water (0.16 mL), 15% sodium hydroxide (0.16 ml) and water (0.48 mL) were successively added, and the mixture was stirred at room temperature for 15 min. The insoluble material was filtered off through celite, and the filtrate was concentrated under reduced pressure. The residue was purified by column chromatography (carrier: silica gel, eluent: hexane-ethyl acetate) to give the title compound (0.64 g) as a solid.

WORKUP

后处理

  1. stirringthe mixture was stirred at room temperature for 15 min
  2. filtrationThe insoluble material was filtered off through celite
  3. concentrationthe filtrate was concentrated under reduced pressure
  4. customThe residue was purified by column chromatography (carrier: silica gel, eluent: hexane-ethyl acetate)