HuagongsheHuagongshe Chemistry Print Report · For research reference only
Diisopropylethylamine → HCID 118387978, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | 1-methyl-1H-pyrazol-4-amine | HCID 4770990 | — |
| Reactant | HCID 118387943 | HCID 118387943 | — |
| Solvent | 1-Butanol | HCID 263 | — |
| Product | HCID 118387978 | HCID 118387978 | 70% |
Reaction Conditions
| Temperature | 150 °C |
|---|
Reaction Steps
To a suspension of 6-((2-chloro-5-methylpyrimidin-4-yl)amino)hexahydrofuro[3,2-b]furan-3-ol (54 mg, 0.20 mmol) in n-BuOH (1 mL) was added 1-methyl-1H-pyrazol-4-amine (32 mg, 0.24 mmol) and DIPEA (78 mg, 0.60 mmol). Then the mixture was stirred under nitrogen atmosphere at 150° C. overnight and concentrated in vacuo. To the residue was added water (20 mL), and extracted with DCM (20 mL×3). The combined organic phases were washed with brine (30 mL), dried over anhydrous Na2SO4, filtered and concentrated in vacuo to give crude oil. Then it was purified by silica gel column chromatography (DCM/MeOH (v/v)=20/1) to give the title compound as an off-white solid (46 mg, 70%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09394281B2 |
| Source dataset | uspto-grants-2016_07 |
| ORD ID | ord-5158fbd8633747c0adbe4f16f5d3a4e2 |
| Source note | uspto-grants-2016_07 |