反応 #53654

反応方程式

diisopropyl ether

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

hydrochloric acid

sodium hydrogencarbonate

→

1H-indazol-5-yl 3-fluorobenzenesulfonate

収率 59.3%

溶媒

water

反応条件

後処理

1. 1
   温度to reflux for 16 hours
2. 2
   その他After returning to a temperature in the region of 20° C.
3. 3
   抽出extracted with two times 10 ml of dichloromethane
4. 4
   乾燥The pooled organic extracts are dried over calcium chloride
5. 5
   ろ過filtered
6. 6
   濃縮concentrated by evaporation under reduced pressure
7. 7
   その他The transluscent oil obtained
8. 8
   濃縮concentrated by trituration
9. 9
   その他The solid obtained
10. 10
    その他is separated by filtration
11. 11
    洗浄washed with two times 1 ml of diisopropyl ether
12. 12
    その他dried under reduced pressure

実験手順

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).

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