反应详情

Combine 0.5 g (1 mmol) of 1-[cis-4-(tert-butyl-dimethyl-silanyloxy)-cyclohexyl]-3-(2,6-dichloro-4-hydroxy-benzyl)-pyrrolidin-2-one (Preparation 72) 0.7 g (2 mmol) Cs2CO3 and 0.49 g (3 mmol) p-fluoromethylbenzoate in 10 mL dry DMF and heat at 100° C. for 4 hours. Dilute the mixture with 25 mL H2O and 50 mL EtOAc. Separate the layers and extract the aqueous with 50 mL EtOAc. Combine the organic layers, wash with brine, dry over MgSO4 and concentrate under vacuum. Purify via chromatography using 30% EtOAc in hexanes to recover 0.47 g of an oil.

1. customSeparate the layers
2. extractionextract the aqueous with 50 mL EtOAc
3. washwash with brine
4. dry with materialdry over MgSO4
5. concentrationconcentrate under vacuum
6. customPurify via chromatography
7. customto recover 0.47 g of an oil