HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 53966919, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Tert-Butyl nitrite | HCID 10906 | — |
| Reactant | 2-Benzothiazolamine, dichloro- | HCID 112722 | — |
| Reactant | Sodium Bromide | HCID 253881 | — |
| Catalyst | copper(I) bromide | HCID 24593 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | HCID 53966919 | HCID 53966919 | — |
Reaction Steps
35 g (0.24 mol) of copper(I) bromide and 126 g (1.23 mol) of sodium bromide were added to a solution of 27 g (0.12 mol) of 2-amino-4,6-dichlorobenzothiazole in 0.5 1 of acetonitrile, and 16.5 g (0.16 mol) of tert-butyl nitrite were then added dropwise. Stirring was carried out for 16 hours, after which the reaction mixture was acidified with 10% strength hydrochloric acid. The product was then extracted with methyl tert-butyl ether. The organic phase was washed with water, dried over magnesium sulfate and finally evaporated down. Purification of the crude product was carried out by means of column chromatography over silica gel (eluent: 1:1 cyclohexane/ethyl acetate). Yield: 9.1 g.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05888940 |
| Source dataset | uspto-grants-1999_03 |
| ORD ID | ord-bb9b974847924fa3aea17c3b8330233b |
| Source note | uspto-grants-1999_03 |