反应详情

温度

45 °C

11-Acetyl-4-formyl-6,9-dihydroxy-14-oxa-1,11-diazatetracyclo[7.4.1.02,7.010,12 ]tetradeca-2,4,6-trien-8-ylmethyl carbamate (55 mg) was dissolved in a mixture of acetone (2 ml) and methyl iodide (2 ml). To the solution was added potassium carbonate (150 mg), and the mixture was stirred at 45° C. overnight under nitrogen atmosphere. The mixture was cooled to room temperature and filtered, and the filter cake was washed with a mixture of chloroform and acetone (1:1, v/v, 10 ml). The filtrate and the washings were combined and evaporated in vacuo. The residue was subjected to column chromatography on silica gel, and elution was carried out with a mixture of chloroform and acetone (4:1, v/v). The desired fractions were collected and evaporated to dryness. The residue was subjected to preparative thin layer chromatography, which was developed with a mixture of chloroform and methanol (1:1, v/v) to afford 11-acetyl-4-formyl-9-hydroxy-6-methoxy-14-oxa-1,11-diazatetracyclo[7.4.1.02,7.010,12 ]tetradeca-2,4,6-trien-8-ylmethyl carbamate (11 mg).

1. temperatureThe mixture was cooled to room temperature
2. filtrationfiltered
3. washthe filter cake was washed with a mixture of chloroform and acetone (1:1, v/v, 10 ml)
4. customevaporated in vacuo
5. washThe residue was subjected to column chromatography on silica gel, and elution
6. additionwas carried out with a mixture of chloroform and acetone (4:1
7. customThe desired fractions were collected
8. customevaporated to dryness
9. additionwas developed with a mixture of chloroform and methanol (1:1