HuagongsheHuagongshe Chemistry Print Report · For research reference only
Diisopropylethylamine → [1-(2-Chloro-6,7-dihydrothieno[3,2-d]pyrimidin-4-ylamino)-cyclopropyl]-methanol
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | (1-Aminocyclopropyl)methanol | HCID 14146220 | — |
| Reactant | 2,4-Dichloro-6,7-dihydrothieno[3,2-d]pyrimidine | HCID 45789967 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | [1-(2-Chloro-6,7-dihydrothieno[3,2-d]pyrimidin-4-ylamino)-cyclopropyl]-methanol | HCID 59708441 | — |
Reaction Conditions
| Temperature | 160 °C |
|---|
Reaction Steps
1.4 g (II) are placed in 10 ml dioxane, then 3.6 ml diisopropylethylamine are added followed by 1 g 1-aminocyclopropanmethanol (cf. 2.2). The reaction mixture is heated to 160° C. until there is no further reaction, then cooled and evaporated down. The residue is treated with cyclohexane/ethyl acetate (4:1) in the ultrasound bath, the solid is suction filtered and dried. 1.24 g (III-2) are obtained in the form of a solid. Analytical HPLC-MS (method A): RT=1.01 min.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09161927B2 |
| Source dataset | uspto-grants-2015_10 |
| ORD ID | ord-c17f035adf854abc919f0509632daf9d |
| Source note | uspto-grants-2015_10 |