Triethylamine → Methanesulfonic acid 4-(2,6-dioxo-1,3-dipropyl-2,3,6,7-tetrahydro-1H-purin-8-yl)-bicyclo[2.2.2]oct-1-yl ester

To a solution of 50 mg of 8-(4-Hydroxy-bicyclo[2.2.2]oct-1-yl)-1,3-dipropyl-3,7-dihydro-purine-2,6-dione (Example 13a) (0.14 mmol) in CH2Cl2 (5 ml) was added 20 μL of Et3N and the reaction mixture cooled in an ice bath. To this was added 20 μL of methanesulfonyl chloride (0.26 mmol) and the reaction mixture kept at 10° C. overnight. The reaction mixture was concentrated in vacuo and the residue taken up in EtOAc and washed 2× with dilute HCl (5 ml). The organic layer was dried over NaSO4 and conc'd. The residue was triturated in acetonitrile to afford 36 mg (59%) of pure white solid (MH+=439.4).

1. temperaturethe reaction mixture cooled in an ice bath
2. concentrationThe reaction mixture was concentrated in vacuo
3. washwashed 2× with dilute HCl (5 ml)
4. dry with materialThe organic layer was dried over NaSO4 and conc'd
5. customThe residue was triturated in acetonitrile

ORDレコード

ord-520dcee7e5894143af209ac4b0c1b0b8

出典データセット

uspto-grants-2003_11

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US06649600B1