反应详情

温度

100 °C

A mixture of 7-chloromethyl-2-(naphthalene-1-sulfonyl)-7,8-dihydro-6-oxa-1,8a-diaza-acenaphthylene (0.075 g, 0.18 mmoles) and dimethylamine (0.56 ml, 1M solution in THF, 0.56 mmoles) in DMSO was stirred under nitrogen at 100° C. for 4 hours, cooled to room temperature, diluted with water and extracted with EtOAc. The extracts were combined, washed sequentially with water and brine, dried over Na2SO4 and concentrated under vacuum. The resultant residue was purified by flash chromatography using as eluent 5% CH3OH/EtOAc. The purified compound was dissolved in methanol, treated with 1M HCl in ether (0.2 ml, 0.2 mmoles) and evaporated to dryness to afford the title compound, MS: (ES) m/z 407.

1. temperaturecooled to room temperature
2. extractionextracted with EtOAc
3. washwashed sequentially with water and brine
4. dry with materialdried over Na2SO4
5. concentrationconcentrated under vacuum
6. customThe resultant residue was purified by flash chromatography
7. dissolutionThe purified compound was dissolved in methanol
8. customevaporated to dryness