反应详情

温度

80 °C

To 10 mL DCE was added 533 mg (3.7 mmol) phosphorus pentoxide and 1.57 mL (7.36 mmol) bis-trimethylsilyl ether and the mixture was heated at 80° C. for 15 minutes. 0.19 g (0.92 mmol) N-boc-azetidine-3-carboxylic acid and 108 μL (1.01 mmol) 2-aminothiophenol were added and the mixture heated at 85° C. for 20 minutes. After cooling to room temperature the mixture was diluted with 20 mL DCM and washed with 1 M Na2CO3 (2×10 mL). The organic layer was dried with Na2SO4. After filtration and evaporation of the solvent the product was purified by column chromatography (silica, hexane/EtOAc 1:1).

1. temperaturethe mixture heated at 85° C. for 20 minutes
2. temperatureAfter cooling to room temperature the mixture
3. washwashed with 1 M Na2CO3 (2×10 mL)
4. dry with materialThe organic layer was dried with Na2SO4
5. filtrationAfter filtration and evaporation of the solvent the product
6. customwas purified by column chromatography (silica, hexane/EtOAc 1:1)