HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dimethylformamide diethylacetal → 3-(Dimethylamino)-2-pyridin-3-yl-acrylic acid ethyl ester
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dimethylformamide diethylacetal | HCID 70913 | — |
| Reactant | Ethyl 3-pyridylacetate | HCID 96490 | — |
| Product | 3-(Dimethylamino)-2-pyridin-3-yl-acrylic acid ethyl ester | HCID 68704864 | — |
Reaction Steps
37.4 g (226 mmol) pyridin-3-ylacetic acid ethyl ester are heated in 100 g (679 mmol) dimethylformamide diethyl acetal overnight at 100° C. After cooling, the mixture is concentrated and the residue is pre-purified by means of flash chromatography on silica gel (mobile phase: gradient cyclohexane/ethyl acetate 1:1→ethyl acetate/ethanol 9:1). The product obtained is subjected to fine purification by vacuum distillation (1 mbar, 200° C. bath temperature).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09085572B2 |
| Source dataset | uspto-grants-2015_07 |
| ORD ID | ord-51e86c00346f48599f06eaa5efbfaf91 |
| Source note | uspto-grants-2015_07 |