تفاعل #1914818

معادلة التفاعل

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

المذيبات

N,N-dimethylacetamide

ظروف التفاعل

المعالجة

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

الإجراء التجريبي

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).

المصدر