反应详情

温度

50 °C

2.3 g of (5-hydroxy-2-oxopentyl)triphenylphosphorane was dissolved in methylene chloride and extracted 4 times with aqueous hydrochloric acid (pH 1 to 2) and the extracts were combined, sodium chloride added and then extracted with methylene chloride (4×50 ml). The organic extracts were combined, dried over sodium sulfate, and the solvent removed under nitrogen gas followed by heating to 50° C./0.5 mm Hg for 6 hours and crystallization from acetone to give 1.9 g of product, m.p. 143°-145° C. identical with that obtained by the process in Example 10.

1. extractionextracted 4 times with aqueous hydrochloric acid (pH 1 to 2)
2. additionsodium chloride added
3. extractionextracted with methylene chloride (4×50 ml)
4. dry with materialdried over sodium sulfate
5. customthe solvent removed under nitrogen gas
6. customcrystallization from acetone