反応 #1914818

反応方程式

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

溶媒

N,N-dimethylacetamide

反応条件

後処理

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

実験手順

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).

出典