HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrazine → HCID 71516705, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrazine | HCID 9321 | — |
| Reactant | HCID 89443778 | HCID 89443778 | — |
| Solvent | Dimethyl Sulfoxide | HCID 679 | — |
| Product | HCID 71516705 | HCID 71516705 | 99.8% |
Reaction Steps
The 3-bromo-4,6-dimethylthieno[2,3-b]pyridine-2-carbonitrile (1.11 g, 4.17 mmol) was added to a microwave reaction vial. The DMSO (14 mL) was added, followed by hydrazine (0.392 mL, 12.5 mmol). The vial was sealed and irradiated at 150 degrees for 10 minutes. LCMS showed no remaining starting material. The reaction was cooled to RT, then poured into 150 mL of ice-water. The ice was allowed to melt and resulting slurry was poured through filter paper, washing the solid with cold water (3×). The solid was then dried under vacuum at 60° C. to give 908 mg (98%) of the product as a light yellow solid. 1H NMR (400 MHz, DMSO-d6): δ ppm 7.07 (s, 1H), 5.35 (bs, 2H), 2.62 (s, 3H), 2.49 (s, 3H). LC/MS: RT=0.38 min., m/z=219.0 [M+H]+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09056876B2 |
| Source dataset | uspto-grants-2015_06 |
| ORD ID | ord-a4bfb462fea84b77bf3f9a9d32096cc6 |
| Source note | uspto-grants-2015_06 |