HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Acetate → HCID 11630741, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Acetate | HCID 517045 | — |
| Reactant | 4-Methoxyphenylhydrazine hydrochloride | HCID 2723904 | — |
| Reactant | 6-(1,3-Dioxopropan-2-yl)picolinic acid | HCID 2735204 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Product | HCID 11630741 | HCID 11630741 | 61% |
Reaction Steps
A solution of 6-(diformylmethyl)-pyridin-2-carboxylic acid (315 mg, 1.63 mmol), 4-methoxyphenylhydrazine hydrochloride (285 mg, 1.63 mmol) and sodium acetate (134 mg, 1.63 mmol) in acetic acid (5 mL) is heated to 110° C. for 18 h. After being allowed to cool, the solution is filtered. The solid product is washed with ethyl acetate and diethyl ether, and dried under vacuum to afford the title product (294 mg, 0.99 mmol, 61%) as a beige powder. m.p. 122-123° C. 1H NMR (300 MHz, DMSO-d6): δ 9.11 (1H, s), 8.38 (1H, s), 7.99 (2H, d, J=4.7 Hz), 7.86 (1H, t, J=4.4 Hz), 7.80 (2H, d, J=9.1 Hz), 7.08 (2H, d, J=9.1 Hz), 3.80 (3H, s), 1H missing. MS (ES+): m/e 297 (18), 296 (100). MS (ES−): m/e 295 (14), 294 (100).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09051342B2 |
| Source dataset | uspto-grants-2015_06 |
| ORD ID | ord-ead393ce1a5147838c4fe00b3a13a71c |
| Source note | uspto-grants-2015_06 |