反应详情

Sulfone 11.1 (350 mg, 104 mmol) was combined with 4-aminocyclohexylmethanol 1:1 cis/trans) (400 mg, 3.3 mmol) (prepared as described in Chem.Ber.; GE; 96; 1963; 2377-2386) with 0.3 mL of 1-methyl-2-pyrrolidinone. The mixture was heated at 1000 for 2 hours at which time it was cooled to room temperature. The reaction mixture was added to water and extracted with ethyl acetate, washed with water, dried, and concentrated in vacuo. The residue was purified by column chromatography on silica gel using 10:90 methanol/dichloromethane as eluant The column fractions containing the product were concentrated to a foam which was resuspended in methanol. Addition of hydrochloric acid (1.0M/Et2O, 1.0 equivalent) gave a salt which was filtered to give the hydrochloride salt of 3-(2-chlorophenyl)-7-(4-hydroxymethylcyclohexylamino)-3,4-dihydropyrimido[4,5-d]pyrimidin-2(1H)-one.

1. temperatureThe mixture was heated at 1000 for 2 hours at which time it
2. extractionextracted with ethyl acetate
3. washwashed with water
4. customdried
5. concentrationconcentrated in vacuo
6. customThe residue was purified by column chromatography on silica gel using 10:90 methanol/dichloromethane as eluant The column fractions
7. additioncontaining the product
8. concentrationwere concentrated to a foam which
9. customgave a salt which
10. filtrationwas filtered