反应详情

To a stirring solution of sodium tert.-butoxide (13.45 g) in DME (80 ml) was added dropwise under nitrogen a solution of 2-cyclopropylethanol (12.1 g) in DME (40 ml) over 5 min. After 30 min 2-chloro-9-(tetrahydro-2H-pyran-2-yl)-9H-purin-6-amine (11.84 g) was added and the stirring mixture refluxed for 20 h. After cooling the mixture was treated with water and extracted twice with ethyl acetate. The combined extracts were washed with water then brine, dried by passing through a hydrophobic frit and evaporated to a brown oil. This was re-evaporated twice from toluene then purified on a silica column using an ISCO Companion, eluting with methanol:ethyl acetate (0-12%) to give the title compound. Yield 6.53 gm.

1. temperaturethe stirring mixture refluxed for 20 h
2. temperatureAfter cooling the mixture
3. extractionextracted twice with ethyl acetate
4. washThe combined extracts were washed with water
5. dry with materialbrine, dried
6. customevaporated to a brown oil
7. customThis was re-evaporated twice from toluene
8. customthen purified on a silica column
9. washeluting with methanol