HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 22129651, compound → HCID 178503308, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 22129651 | HCID 22129651 | — |
| Reactant | Sodium Nitrite | HCID 23668193 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 178503308 | HCID 178503308 | — |
Reaction Steps
A SOLUTION OF SODIUM NITRITE (842 MG, 12.2 MMOL) IN WATER (100 ML) WAS ADDED TO A STIRRED SOLUTION OF 3-AMINO-2-BROMO-5-METHYLTHIOPYRAZINE (2.44 G, 11.1 MMOL) IN ACETIC ACID (100 ML) AT 0°C. THE REACTION WAS WARMED TO RT AND AFTER 16 H THE REACTION MIXTURE WAS PARTITIONED BETWEEN WATER AND METHYLENE CHLORIDE. THE ORGANIC LAYER WAS DRIED (NA2SO4) AND EVAPORATED IN VACUO. THE CRUDE PRODUCT WAS PURIFIED BY FLASH COLUMN CHROMATOGRAPHY ON SILICA GEL (40% ETHYL ACETATE/HEXANES) TO GIVE THE TITLE COMPOUND AS A CRYSTALLINE SOLID:
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06147078 |
| Source dataset | uspto-grants-2000_11 |
| ORD ID | ord-647481653fba4845b06134a4f577982e |
| Source note | uspto-grants-2000_11 |