반응 #12013
ord-b9de31a32fdc4c3f897713ad2e8c473b
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후처리
- 1기타After a solution had formed
- 2온도the reaction mixture was heated to 180 deg C
- 3여과the suspension was filtered through a bed of dicalite speed plus
- 4기타The phases were separated
- 5세척the aqueous layer was washed with ethyl acetate
- 6세척the combined organic phases were washed with brine
- 7건조dried over magnesium sulfate
- 8여과filtered
- 9기타evaporated
- 10기타The residue was purified by chromatography over silica gel (0.032–0.063 mm) with tert-butyl methyl ether:n-hexane (1:5) as eluant
실험 절차
To a solution of 0.8 g (2.17 mmol) (4R,9aR)-6-bromo-4-methyl-3,4,9,9a-tetrahydro-1H-2,4a,5-triaza-fluorene-2-carboxylic acid tert-butyl ester (Example 5, intermediate b) in 12 ml 1-methyl-2-pyrrolidone, 2.36 g (17.4 mmol) sodium trifluoroacetate was added. After a solution had formed, 1.65 g (8.7 mmol) copper iodide was added and the reaction mixture was heated to 180 deg C. for 2 h. The mixture was cooled to room temperature, ethyl acetate and water were added and the suspension was filtered through a bed of dicalite speed plus. The phases were separated, the aqueous layer was washed with ethyl acetate and the combined organic phases were washed with brine, dried over magnesium sulfate, filtered and evaporated. The residue was purified by chromatography over silica gel (0.032–0.063 mm) with tert-butyl methyl ether:n-hexane (1:5) as eluant to afford the desired compound as a colorless oil (27.7%).