反应详情

温度

0 °C

Under an inert atmosphere, 0.60 g (2.49 mmoles) of tert-butyl 2-hydroxy-7-aza-spiro[3.5]-nonane-7-carboxylate (WO 2003084948) is dissolved in 25 ml of toluene. 1.024 g (3.90 mmoles) of triphenylphosphine and 0.384 g (2.98 mmoles) of 4-chlorophenol are added. The medium is cooled to 0° C., then a solution of 0.528 g (3.03 mmoles) of diethylazodicarboxylate in 3 ml of toluene is added. The medium is stirred for 14 hrs at ambient temperature then concentrated under vacuum. The residue obtained is taken up in a saturated aqueous solution of sodium carbonate and extracted twice with dichloromethane. The combined organic phases are washed once with a saturated aqueous solution of sodium chloride, dried over sodium sulphate, filtered and concentrated under vacuum. 0.874 g of a residue is obtained, which is used as such in the following stage.

1. concentrationthen concentrated under vacuum
2. customThe residue obtained
3. extractionextracted twice with dichloromethane
4. washThe combined organic phases are washed once with a saturated aqueous solution of sodium chloride
5. dry with materialdried over sodium sulphate
6. filtrationfiltered
7. concentrationconcentrated under vacuum