Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Sulfamic Acid | HCID 5987 | — |
| Reactant | 5-Tetralinylamine | HCID 16671 | — |
| Solvent | 1,2-Dichlorobenzene | HCID 7239 | — |
| Solvent | N-methyl-2-pyrrolidone | HCID 13387 | — |
| Product | HCID 11447496 | HCID 11447496 | 48.6% |
Reaction Steps
A hot suspension of 20 g of sulphamic acid in 40 ml of N-methylpyrrolidone is added to a solution of 10 g of 5,6,7,8-tetrahydronaphthylamine in 100 ml of 1,2-dichlorobenzene. The mixture is heated with stirring for 7 hours at 150° C. The product is filtered off and washed with dichlorobenzene and then with toluene. The precipitate is resuspended in 70 ml of water and neutralized to pH 7 with 5.5 ml of 30% sodium hydroxide. The insoluble matter is filtered off and the aqueous phase is extracted with ether. The aqueous phase is adjusted to pH 5 by adding HCl, at 5° C.; the mixture is filtered, and the residue is washed with water and dried to obtain 7.5 g of the expected product.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US05925661 |
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| Source dataset | uspto-grants-1999_07 |
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| ORD ID | ord-4abdbeb762474c8888646d4d598df885 |
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| Source note | uspto-grants-1999_07 |
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