HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → Methyl N-[(1S)-2-[[4-[3-iodo-1-(1-methylethyl)-1H-pyrazol-4-yl]-2-pyrimidinyl]amino]-1-methylethyl]carbamate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | 2-Chloro-4-(3-iodo-1-(1-methylethyl)-1H-pyrazol-4-yl)pyrimidine | HCID 51034341 | — |
| Reactant | (S)-methyl 1-aminopropan-2-ylcarbamate | HCID 71721514 | — |
| Solvent | Isopropanol | HCID 3776 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | Methyl N-[(1S)-2-[[4-[3-iodo-1-(1-methylethyl)-1H-pyrazol-4-yl]-2-pyrimidinyl]amino]-1-methylethyl]carbamate | HCID 51034342 | — |
Reaction Steps
A solution of Intermediate 2-chloro-4-(3-iodo-1-isopropyl-1H-pyrazol-4-yl)pyrimidine (1.4 g, 4.01 mmol), (S)-methyl 1-aminopropan-2-ylcarbamate (0.8 g, 6 mmol) and triethylamine (2.8 ml, 20 mmol) in isopropanol (30 ml) and dioxane (20 mL) was heated in a sealed vessel at 125° C. for 48 hours. The cooled mixture was concentrated under vacuum, and aqueous sodium bicarbonate was added to the residue. The mixture was extracted with ethyl acetate, and the combined extracts were dried over sodium sulfate, filtered, and concentrated. The crude residue was purified by silica gel column chromatography (1:2 hexanes/ethyl acetate eluant) to provide the title compound as a white solid. MS m/z 445.0 (M+1).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08501758B2 |
| Source dataset | uspto-grants-2013_08 |
| ORD ID | ord-1839d3898b0e42348a5efe1de7dece5d |
| Source note | uspto-grants-2013_08 |