反应详情

Sodium hydride (1.6 mg, 60% in oil) was added to trans-N-(7-chloro-2,3,4,14b-tetrahydro-1H-dibenzo[b,f]pyrido[1,2-d][1,4]oxazepin-1-yl)-2,2,2-trifluoroacetamide (15 mg, 0.04 mmol) in 1 mL of DMF. After 10 minutes stirring methyl iodide (2.47 μL, 0.04 mmol) was added. The resulting mixture was stirred at room temperature for 18 h. After evaporation the crude compound was purified by chromatography on silica. Elution with toluene/ethyl acetate 7:3 gave trans-N-(7-chloro-2,3,4,14b-tetrahydro-1H-dibenzo[b,f]pyrido[1,2-d][1,4]oxazepin-1-yl)-2,2,2-trifluoro-N-methylacetamide (14 mg, 90%). Data: (m/z)=411 (M+H)+.

1. additionwas added
2. customAfter evaporation the crude compound
3. customwas purified by chromatography on silica
4. washElution with toluene/ethyl acetate 7:3