HuagongsheHuagongshe Chemistry Print Report · For research reference only
Diisopropylethylamine → HCID 59708434, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | D-Valinol | HCID 6950587 | — |
| Reactant | 2,4-Dichloro-6,7-dihydrothieno[3,2-d]pyrimidine | HCID 45789967 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 59708434 | HCID 59708434 | — |
Reaction Conditions
| Temperature | 100 °C |
|---|
Reaction Steps
7.2 g 2,4-dichloro-6,7-dihydrothieno[3,2-d]pyrimidine (II) are placed in 36 ml dioxane, then first 18 ml diisopropylethylamine are added, followed by 6.1 g (R)-(−)-2-amino-3-methyl-1-butanol. The reaction mixture is heated to 100° C. until there is no further reaction, then cooled and evaporated down. The residue is treated with petroleum ether/ethyl acetate (9:1) in the ultrasound bath and the solid is suction filtered and dried. 8.3 g (III-1) are obtained in the form of a solid. Analytical HPLC (method A): RT=2.75 min
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09161927B2 |
| Source dataset | uspto-grants-2015_10 |
| ORD ID | ord-4b322a89a9b04f5f9c222b2ee87c658b |
| Source note | uspto-grants-2015_10 |