HRID1673173

反应详情

EQUATION

反应方程式

HRID 1673173 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
65 °C

PROCEDURE

实验过程

(R)-6-fluoro-3,4-dihydro-2-((R)-2,2-dimethyl-1,3-dioxolan-4-yl)-2H-chromene (2.92 g, 11.6 mmol) was dissolved in acetic acid (24 ml) and demi water (9 ml). The reaction mixture was stirred vigorously and heated to 65° C. After 3 h at 65° C. the reaction mixture was cooled to 25° C. The solution was then concentrated in vacuo to obtain a vetrous oil. Chromatographic separation on silica of the crude, using a mixture of heptane:ethyl acetate 1:1 as eluent, furnished 0.64 g of (R)-1-((R)-6-fluoro-3,4-dihydro-2H-chromen-2-yl)ethane-1,2-diol as a white solid (26% yield).

WORKUP

后处理

  1. temperatureAfter 3 h at 65° C. the reaction mixture was cooled to 25° C
  2. concentrationThe solution was then concentrated in vacuo
  3. customto obtain a vetrous oil
  4. customChromatographic separation on silica of the crude
  5. additiona mixture of heptane:ethyl acetate 1:1 as eluent