HuagongsheHuagongshe Chemistry Print Report · For research reference only
1,2,3,4-Tetrahydroisoquinoline → 4-[1-tert-Butoxycarbonyl-2-(3,4-dihydro-1H-isoquinoline-2-sulfonyl)-ethyl]-piperidine-1-carboxylic acid benzyl ester
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1,2,3,4-Tetrahydroisoquinoline | HCID 7046 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | 4-(1-Tert-butoxycarbonyl-2-chlorosulfonyl-ethyl)-piperidine-1-carboxylic acid benzyl ester | HCID 86584275 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | 4-[1-tert-Butoxycarbonyl-2-(3,4-dihydro-1H-isoquinoline-2-sulfonyl)-ethyl]-piperidine-1-carboxylic acid benzyl ester | HCID 69748522 | 83% |
Reaction Steps
1,2,3,4-Tetrahydroisoquinoline (0.17 ml) was dissolved in dichloromethane (40 ml) at room temperature under nitrogen. Triethylamine (0.19 ml) was added, followed by 4-(1-tert-butoxycarbonyl-2-chlorosulfonyl-ethyl)-piperidine-1-carboxylic acid benzyl ester (500 mg) as a solution in dichloromethane (1.5 ml). The reaction was left to stir for 64 h then diluted with dichloromethane (60 ml), washed with 10% citric acid solution (2×50 ml), water (2×50 ml), saturated sodium bicarbonate solution (2×50 ml) and brine (50 ml). The organic layer was then dried (MgSO4), filtered and the solvent removed under reduced pressure to give the title compound (506 mg, 83%) as a yellow oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06506773B2 |
| Source dataset | uspto-grants-2003_01 |
| ORD ID | ord-8589a9f96f6542c2bfb3d092c4e35a4d |
| Source note | uspto-grants-2003_01 |