반응 #1914818

반응 방정식

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

용매

N,N-dimethylacetamide

반응 조건

후처리

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

실험 절차

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).

출처