Cesium carbonate → HCID 13477569, compound

A 20% aqueous solution of cesium carbonate was slowly added to a mixture of 14.2 g of 10 in 230 ml of methanol and 23 ml of water, until the mixture was neutral (about 50 ml of the carbonate solution). The solvent was evaporated under reduced pressure. The residue was placed in 50 ml of dimethylformamide and stripped twice. The residue was placed in 150 ml of dimethylformamide and 50 ml of methyl iodide was added to the mixture, which then was stirred overnight at room temperature. The mixture was filtered, and a large volume of methylene chloride was added to the filtrate. The filtrate was washed with a large volume of water, dried (Na2SO4) and the solvent was evaporated under reduced pressure. The residue was triturated with hexane, the mixture was filtered, and the solvent was evaporated from the filtrate to give 13, as a tan solid, m.p.: 46°-48° C.

1. customThe solvent was evaporated under reduced pressure
2. addition50 ml of methyl iodide was added to the mixture, which
3. filtrationThe mixture was filtered
4. additiona large volume of methylene chloride was added to the filtrate
5. washThe filtrate was washed with a large volume of water
6. dry with materialdried (Na2SO4)
7. customthe solvent was evaporated under reduced pressure
8. customThe residue was triturated with hexane
9. filtrationthe mixture was filtered
10. customthe solvent was evaporated from the filtrate

ORD record

ord-20f084c2beef483e97e2ee7abcd25ffa

Source dataset

uspto-grants-1985_07

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US04528028