反应详情

1,1-Dioxo-1λ6-thiomorpholine-4-carbonyl chloride (51.4 mg; 0.26 mmol) is added to a mixture of (S)-Azetidine-2-carboxylic acid (3-tert-butyl-isoxazol-5-yl)-amide; hydrochloride (69 mg; 0.265 mmol) and N,N-diisopropylethylamine (0.141 mL; 0.81 mmol) in THF (2 mL). The reaction mixture is stirred at room temperature for 2 hours. After this time, the reaction mixture is diluted with dichloromethane and washed with water. The layers are separated and the aqueous layer is extracted with dichloromethane once. The organics are combined and washed with brine, dried over Na2SO4, filtered and concentrated in vacuo. Purification by flash chromatography on silica gel using methanol/methylene chloride provides the title compound, m/z 385 [M+H+].

1. washwashed with water
2. customThe layers are separated
3. extractionthe aqueous layer is extracted with dichloromethane once
4. washwashed with brine
5. dry with materialdried over Na2SO4
6. filtrationfiltered
7. concentrationconcentrated in vacuo
8. customPurification by flash chromatography on silica gel