反应详情

A sample of the compound from step 4a (790 mg, 4.48 mmole) was dissolved in 30 mL of THF and 6 mL of water, triphenylphosphine (5.0 g, 19.1 mmole) was added, and the reaction mixture was stfired for 24 hours at reflux. The solvent was removed, and the residue was dissolved in 2 N HCl. NaCl was added, and the solution was extracted with ethyl ether. The aqueous layer was adjusted to pH 12 with K2CO3, saturated with NaCl, then extracted with GICl3 and CHCl3 containing 15% isopropanol. The solvent was removed under vacuum to afford 439 mg of the title compound. MS m/z (M+H)+: 151, MS m/z (M+NH4)+: 168.

1. temperatureat reflux
2. customThe solvent was removed
3. dissolutionthe residue was dissolved in 2 N HCl
4. additionNaCl was added
5. extractionthe solution was extracted with ethyl ether
6. extractionextracted with GICl3 and CHCl3 containing 15% isopropanol
7. customThe solvent was removed under vacuum