Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Ethyl Acetate | HCID 8857 | — |
| Reactant | Sodium ethanethiolate | HCID 4459711 | — |
| Reactant | HCID 67386328 | HCID 67386328 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 59244954 | HCID 59244954 | 43.5% |
Reaction Steps
A solution of 4-(3-methoxyphenyl)-2-morpholin-4-yl-8-pyrimidin-4-yl-5,6,7,8-tetrahydropyrido[2,3-d]pyrimidine (0.50 g, 1.24 mmol) in dimethylformamide (5 ml) was heated to 150° C., and sodium ethanethiolate (1.04 g, 12.4 mmol) was added for every 15 minutes in 3 portions. After heating at 150° C. for 2 hours, sodium ethanethiolate (1.04 g, 12.4 mmol) was added, followed by heating for further 15 minutes. After cooling the reaction mixture, water (5 ml) and ethyl acetate (20 ml) were added, to filter off the deposited precipitate. The crude product was purified by silica column chromatography (dichloromethane/methanol=95/5), to obtain the desired compound as a pale brown solid (0.21 g, 43% yield).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US08022205B2 |
|---|
| Source dataset | uspto-grants-2011_09 |
|---|
| ORD ID | ord-668b0381dcaf4c2d8bef9d4d94bbe3a4 |
|---|
| Source note | uspto-grants-2011_09 |
|---|