(S)-7-Amino-6,7-dihydro-9H-5-oxa-9-aza-benzocyclohepten-8-one

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: To a solution of 0.07 g (0.37 mmol) (S)-7-amino-6,7-dihydro-9H-5-oxa-9-aza-benzocyclohepten-8-one in 7 ml tetrahydrofurane were added 0.15 g (0.59 mmol) 2-methyl-N-(2,2,3,3,3-pentafluoro-propyl)-malonamic acid, 0.09 g (0.59 mmol) 1-hydroxybenzotriazole hydrate, 0.12 g (0.59 mmol) N-(3-dimethylaminopropyl)-N′-ethyl-carbodiimid-hydrochloride and 1.0 ml (5.9 mmol) diisopropylethylamine. After stirring at room temperature over night the solvent was removed by distillation and the residue was purified by chromatography on silicagel with ethylacetate/heptane (gradient 0–80/100–20) to yield 0.06 g (23%) 2-methyl-N-((S)-8-oxo-6,7,8,9-tetrahydro-5-oxa-9-aza-benzocyclohepten-7-yl)-N′-(2,2,3,3,3-pentafluoro-propyl)-malonamide as light yellow solid, MS m/e (%): 410.3 (M+H+, 100). was removed by distillation the residue was purified by chromatography on silicagel with ethylacetate/heptane (gradient 0–80/100–20)