反应详情

814 mg (2 eq-3.206 mmol) of iodine and 180 mg (2 eq-3.206 mmol) of ground potassium hydroxide are added to a solution of 430 mg (1 eq-1.603 mmol) of (1-acetyl-1H-indazol-5-yl)phosphonic acid dimethyl ester in 20 ml of dimethylformamide. The medium is stirred at ambient temperature over a weekend. Another portion of 814 mg of iodine and 180 mg of potassium hydroxide are added to the reaction mixture, which is continued to stir for an additional period of 3 hours at ambient temperature. 20 ml of a saturated sodium thiosulfate solution are added and the medium is stirred for 10 minutes. The reaction mixture is washed with 40 ml of water. The aqueous phase is treated with 4 times 50 ml of ethyl acetate. The organic phase is dried over magnesium sulfate and then filtered and the solvent is evaporated off under reduced pressure in a rotary evaporator to obtain 458 mg of (3-iodo-1H-indazol-5-yl)phosphonic acid dimethyl ester.

1. stirringto stir for an additional period of 3 hours at ambient temperature
2. stirringthe medium is stirred for 10 minutes
3. washThe reaction mixture is washed with 40 ml of water
4. additionThe aqueous phase is treated with 4 times 50 ml of ethyl acetate
5. dry with materialThe organic phase is dried over magnesium sulfate
6. filtrationfiltered
7. customthe solvent is evaporated off under reduced pressure in a rotary evaporator