HuagongsheHuagongshe Chemistry Print Report · For research reference only
Isopropylamine → HCID 86629464, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Isopropylamine | HCID 6363 | — |
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | Ethyl 4,6-dichloropyridine-3-carboxylate | HCID 600045 | — |
| Solvent | Dimethylacetamide | HCID 31374 | — |
| Product | HCID 86629464 | HCID 86629464 | — |
Reaction Steps
A stirred solution of ethyl 4,6-dichloronicotinate (1) (10 g, 43.4 mmol), isopropyl amine (8 mL) and DIPEA (8 mL) in DMA (50 mL) were heated at 120° C. in a sealed tube for 3 h. The reaction mixture was concentrated to dryness to remove excess of DMA from the reaction mass. The crude material obtained was purified by column chromatography through silica gel and EtOAC: pet. Ether as eluent to obtain the title compound (2). LC/MS: Acquity BEH C18 2.1×50 mm, 1.8 micron; Solvent A=0.1% TFA in water; Solvent B=0.1% TFA in ACN; gradient 0-100% B over 2 min; retention time: 0.90 min; LCMS (ES-API), m/z 243.7 (M+H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09242975B2 |
| Source dataset | uspto-grants-2016_01 |
| ORD ID | ord-b90db7f3204247a7bca70997a6ea094d |
| Source note | uspto-grants-2016_01 |