تفاعل #2028886

معادلة التفاعل

4-(2-Thienyl)butyric acid

acetic anhydride

phosphoric acid

→

oil

المردود 88.9%

4-keto-4,5,6,7-tetrahydrothianaphthene

المردود 88.9%

المذيبات

water

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةheated
2. 2
   درجة الحرارةto reflux for 3.2 hours
3. 3
   استخلاصextracted with ethyl acetate
4. 4
   غسيلwashed with brine
5. 5
   تجفيفdried over MgSO4
6. 6
   تركيزconcentrated in vacuo

الإجراء التجريبي

4-(2-Thienyl)butyric acid (28.42 g, 167 mmol) was placed in a round bottom flask with acetic anhydride (30 mL) and phosphoric acid (0.6 mL), and heated to reflux for 3.2 hours. The reaction mixture was poured into 100 mL of water, extracted with ethyl acetate, washed with brine, dried over MgSO4, and concentrated in vacuo to give a brown oil (22.60 g) which was vacuum distilled (1 mm Hg, 107°-115° C.) to give a white solid (13.08 g, 51%): mp 34°-40° C.); 1H NMR (CDCl3) 300 MHz 7.29 (d, J=5.2 Hz, 1H), 6.99 (d, J=5.2 Hz, 1H, 2.95 (t, J=6.0 Hz, 2H), 2.47(m, 2H), 2.13(m, 2H). M+H=153.

المصدر