反应 #1914818

反应方程式

2-Hydroxymethyl-2,3-dihydro-thieno[3,4-b][1,4]dioxine-5,7-dicarboxylic acid

ethyl acetate

→

(2,3-dihydro-thieno[3,4-b][1,4]dioxin-2-yl)-methanol

溶剂

N,N-dimethylacetamide

反应条件

后处理

1. 1
   温度after which it was cooled to 25° C
2. 2
   其他the catalyst was removed by filtration
3. 3
   洗涤the filtrate was washed with acidic water
4. 4
   其他Subsequently, the solvent was removed after which pure (2,3-dihydro-thieno[3,4-b][1,4]dioxin-2-yl)-methanol
5. 5
   其他was isolated by vacuum distillation (115–120° C.; 0.05 mm Hg)

实验过程

2-Hydroxymethyl-2,3-dihydro-thieno[3,4-b][1,4]dioxine-5,7-dicarboxylic acid (48 g, 0.184 mol) was dissolved in N,N-dimethylacetamide (500 mL), and Cu2Cr2O7 (8.6 g) and quinoline (15 drops) were added. This mixture was subsequently stirred for 2 hours at 150° C., after which it was cooled to 25° C. It was then poured into ethyl acetate, the catalyst was removed by filtration and the filtrate was washed with acidic water and aqueous, saturated NaCl. Subsequently, the solvent was removed after which pure (2,3-dihydro-thieno[3,4-b][1,4]dioxin-2-yl)-methanol was isolated by vacuum distillation (115–120° C.; 0.05 mm Hg).

来源