HRID1881890

反应详情

EQUATION

反应方程式

HRID 1881890 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

A suspension of sodium borohydride (6.18 g) and DL-tartaric acid (24.5 g) in tetrahydrofuran (250 mL) was stirred at 80° C. for 2 hr. The reaction mixture was cooled to 0° C., ethyl [2-(1,3-dioxolan-2-yl)-1,3-thiazol-5-yl](oxo)acetate (10.49 g) was added, and the mixture was stirred at room temperature for 2 days. The reaction mixture was slowly poured into ice (100 g), and the mixture was extracted with ethyl acetate. The ethyl acetate layer was washed with saturated brine, dried (MgSO9) and concentrated. The obtained residue was subjected to silica gel column chromatography, and the title compound (8.43 g, yield 80%) was obtained as a colorless oil from a fraction eluted with ethyl acetate-hexane (4:1, volume ratio). MS: 260 (MH+).

WORKUP

后处理

  1. temperatureThe reaction mixture was cooled to 0° C.
  2. stirringthe mixture was stirred at room temperature for 2 days
  3. extractionthe mixture was extracted with ethyl acetate
  4. washThe ethyl acetate layer was washed with saturated brine
  5. dry with materialdried (MgSO9)
  6. concentrationconcentrated