HuagongsheHuagongshe Chemistry Print Report · For research reference only
3-(tert-butyloxycarbonyl)-1-chloromethyl-5-nitro-1,2-dihydro-3H-benz[e]indole → HCID 10688060, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 3-(tert-butyloxycarbonyl)-1-chloromethyl-5-nitro-1,2-dihydro-3H-benz[e]indole | HCID 15380413 | — |
| Catalyst | Adams' catalyst | HCID 345198 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 10688060 | HCID 10688060 | 90.7% |
Reaction Steps
A solution of 13 (200 mg, 0.55 mmol) in THF (15 mL) was hydrogenated over PtO2 at 55 psi for 1.5 h. The catalyst was removed, the solvent was evaporated, and the resulting solid was triturated with petroleum ether to give 5-amino-3-(tert-butyloxycarbonyl)-1-(chloromethyl)-1,2-dihydro-3H-benz[e]indole (166 mg, 90%), mp >200° C. 1H NMR [(CD3)2SO] δ 8.01 (d, J=8.4 Hz, 1 H, H-6), 7.64 (d, J=8.3 Hz, 1 H, H-9), 7.45-7.25 (underlying br s, 1 H, H-4), 7.40 (t, J=7.4 Hz, 1 H, H-8), 7.20 (t, J=7.4 Hz, 1 H, H-7), 7.91 (s, 2 H, NH2), 4.11-3.87 (m, 4 H, H-1,2, CHHCl), 3.66 (dd, J=10.5, 8.3 Hz, 1 H, CHHCl), 1.53 (s, 9 H, C(CH3)3).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06130237 |
| Source dataset | uspto-grants-2000_10 |
| ORD ID | ord-ad1a0a2768ec433699d212f66667eb7b |
| Source note | uspto-grants-2000_10 |