反应详情

Triphenylphosphine (1.31 g, 4.98 mmol, 1 eq) is added at room temperature to a suspension of 5-(azidomethyl)-2-(methoxymethyl)-6-(trifluoromethyl)imidazo[2,1-b][1,3,4]thiadiazole a18 (1.45 g, 4.98 mmol, 1 eq) in THF/H2O (18 ml/2 ml). The reaction mixture is stirred at room temperature for 60 h. The solvent is evaporated under reduced pressure, water is added to the residue, the solution is acidified to pH 2 with aqueous 5N HCl, then extracted with Et2O (1×50 ml). The aqueous layer is basified (pH 8) by addition of a Na2CO3 aqueous solution, and extracted with dichloromethane (2×50 ml), the cumulated organics layers are dried over MgSO4, filtered and evaporated under reduced pressure to afford 1-[2-(methoxymethyl)-6-(trifluoromethyl)imidazo[2,1-b][1,3,4]thiadiazol-5-yl]methanamine a19.

1. customThe solvent is evaporated under reduced pressure, water
2. additionis added to the residue
3. extractionextracted with Et2O (1×50 ml)
4. additionby addition of a Na2CO3 aqueous solution
5. extractionextracted with dichloromethane (2×50 ml)
6. dry with materialthe cumulated organics layers are dried over MgSO4
7. filtrationfiltered
8. customevaporated under reduced pressure