HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 21191969, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Bromine | HCID 24408 | — |
| Reactant | 2-Hydroxynaphthalen-3,6-dicarboxylic acid | HCID 9816055 | — |
| Solvent | Dimethyl Sulfoxide | HCID 679 | — |
| Solvent | Chloroform | HCID 6212 | — |
| Product | HCID 21191969 | HCID 21191969 | 97% |
Reaction Steps
2-Hydroxy-3,6-di-hydroxycarbonylnaphthalene (11.8 g) was dissolved in chloroform (300 g) and dimethyl sulfoxide (100 g), followed by ice-cooling. Then, a solution of bromine (8.0 g) and chloroform (50 g) was added dropwise at not more than 5° C. over 2 hours. After continuously stirring for 1 hour, this solution was poured into water (1500 g) dropwise. The deposit was filtered and then washed with water and dispersed in a small amount of methanol. The dispersion was concentrated under reduced pressure at room temperature and then dried under vacuum to obtain 15.1 g of 1-bromo-2-hydroxy-3,6-di-hydroxycarbonylnaphthalene as a whitish brown crystal (DSC analysis value: 145.2° C.).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06252104B1 |
| Source dataset | uspto-grants-2001_06 |
| ORD ID | ord-5b2c30495ec24c74a62f090f2275b322 |
| Source note | uspto-grants-2001_06 |