HuagongsheHuagongshe Chemistry Print Report · For research reference only
Diisopropylethylamine → (5S)-5-[(2-Chloro-6,7-dihydrothieno[3,2-d]pyrimidin-4-yl)amino]-1-methyl-2-piperidinone
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | HCID 28064098 | HCID 28064098 | — |
| Reactant | 2,4-Dichloro-6,7-dihydrothieno[3,2-d]pyrimidine | HCID 45789967 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | (5S)-5-[(2-Chloro-6,7-dihydrothieno[3,2-d]pyrimidin-4-yl)amino]-1-methyl-2-piperidinone | HCID 59708467 | — |
Reaction Conditions
| Temperature | 130 °C |
|---|
Reaction Steps
0.27 g (II) are placed in 3 ml dioxane, then first 0.45 ml diisopropylethylamine are added, followed by 0.25 g (S)-5-amino-1-methylpiperidin-2-one. The reaction mixture is heated to 130° C. until there is no further reaction then cooled and evaporated down. The product is extracted with dichloromethane and purified by chromatography (preparative HPLC, method A). 0.26 g (III-5) are obtained in the form of a solid. Analytical HPLC-MS (method A): RT=1.06 min.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09161927B2 |
| Source dataset | uspto-grants-2015_10 |
| ORD ID | ord-4fdd543004ca4762b4f12193b011c4b3 |
| Source note | uspto-grants-2015_10 |