تفاعل #53654

معادلة التفاعل

diisopropyl ether

1-acetyl-1H-indazol-5yl 3-fluorobenzenesulfonate

hydrochloric acid

sodium hydrogencarbonate

→

1H-indazol-5-yl 3-fluorobenzenesulfonate

المردود 59.3%

المذيبات

water

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةto reflux for 16 hours
2. 2
   أخرىAfter returning to a temperature in the region of 20° C.
3. 3
   استخلاصextracted with two times 10 ml of dichloromethane
4. 4
   تجفيفThe pooled organic extracts are dried over calcium chloride
5. 5
   ترشيحfiltered
6. 6
   تركيزconcentrated by evaporation under reduced pressure
7. 7
   أخرىThe transluscent oil obtained
8. 8
   تركيزconcentrated by trituration
9. 9
   أخرىThe solid obtained
10. 10
    أخرىis separated by filtration
11. 11
    غسيلwashed with two times 1 ml of diisopropyl ether
12. 12
    أخرىdried under reduced pressure

الإجراء التجريبي

1H-Indazol-5-yl 3-fluorobenzenesulfonate can be obtained in the following way: a suspension of 193 mg of 1-acetyl-1H-indazol-5yl 3-fluorobenzenesulfonate and of 0.19 ml of hydrochloric acid (d=1.18) in 1.65 ml of distilled water is brought to reflux for 16 hours. After returning to a temperature in the region of 20° C., the reaction medium is basified to a pH in the region of 8 with a saturated aqueous sodium hydrogencarbonate solution and extracted with two times 10 ml of dichloromethane. The pooled organic extracts are dried over calcium chloride, filtered and concentrated by evaporation under reduced pressure. The transluscent oil obtained is taken up with 2 ml of diisopropyl ether and concentrated by trituration. The solid obtained is separated by filtration, washed with two times 1 ml of diisopropyl ether and dried under reduced pressure. 100 mg of 1H-indazol-5-yl 3-fluorobenzenesulfonate are thus obtained in the form of a whiteish solid melting at 104° C. (analysis C13H9FN2O3S, % calculated C, 53.42; H, 3.10; F, 6.50; N, 9.58; O, 16.42; S, 10.97. % found C, 53.5; H, 2.9; F, 6.2; N, 9.6).

المصدر