HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 89408386, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | Di-tert-butyl dicarbonate | HCID 90495 | — |
| Reactant | HCID 117901401 | HCID 117901401 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 89408386 | HCID 89408386 | 101% |
Reaction Steps
(S)-tert-Butyl(1-(4-chloro-3-fluoropyridin-2-yl)but-3-en-1-yl)(methyl)carbamate: A solution of Intermediate 30A (0.11 g, 0.345 mmol), 4 N HCl in dioxane (3 mL), and MeOH (3.00 mL) was stirred at rt for 1 h. The reaction mixture was concentrated. The residue was re-dissolved in acetonitrile (3.00 mL) and added DIEA (0.241 mL, 1.380 mmol) followed by BOC2O (0.104 mL, 0.449 mmol). The reaction was stirred at rt for 2 h and concentrated. The residue was purified by silica gel chromatography to yield the desired product (0.11 g, 101%). MS (ESI) m/z: 314.9 (M+H)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09108981B2 |
| Source dataset | uspto-grants-2015_08 |
| ORD ID | ord-e47c7e977d5f43e4830192783c527378 |
| Source note | uspto-grants-2015_08 |