HuagongsheHuagongshe Chemistry Print Report · For research reference only
Trifluoroacetic acid → N-(5-aminopentyl)-N-methyl-2-nitrobenzenesulfonamide
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Trifluoroacetic acid | HCID 6422 | — |
| Reactant | tert-butyl 5-(N-methyl-2-nitrophenylsulfonamido)pentylcarbamate | HCID 86652975 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Solvent | Diisopropyl Ether | HCID 7914 | — |
| Product | N-(5-aminopentyl)-N-methyl-2-nitrobenzenesulfonamide | HCID 58244791 | 99.5% |
Reaction Steps
A solution of tert-butyl 5-(N-methyl-2-nitrophenylsulfonamido)pentylcarbamate 30d (31.5 g, 79 mmoles) and trifluoro acetic acid (29.2 mL, 5 eq) in DCM (300 mL) was stirred at RT until completion (˜16 h). The RM was then concentrated under vacuo, redissolved in DCM, washed with a saturated sodium bicarbonate aqueous solution (2 times), then brine, dried over magnesium sulfate, filtered and concentrated. Trituration in diisopropyl ether afforded 23.7 g (quantitative yield) of N-(5-aminopentyl)-N-methyl-2-nitrobenzenesulfonamide 26a as a slightly yellow solid; m/z 302 [M+H]+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09427440B2 |
| Source dataset | uspto-grants-2016_08 |
| ORD ID | ord-4bf96f75660c41a693b59e920940242b |
| Source note | uspto-grants-2016_08 |