HuagongsheHuagongshe Chemistry Print Report · For research reference only
1,4-Dioxane hydrochloride → HCID 86271860, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1,4-Dioxane hydrochloride | HCID 20443148 | — |
| Reactant | HCID 131733445 | HCID 131733445 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 86271860 | HCID 86271860 | — |
Reaction Steps
HCl/dioxane (4N, 5 mL) was added at 0° C. to a solution of tert-butyl (3-(3-(((1,1-dioxidotetrahydro-2H-thiopyran-4-yl)methyl)sulfonyl)phenyl)-3-oxopropyl)carbamate (0.40 g, 0.87 mmol) in CH2Cl2 (10 mL) and the reaction mixture was stirred at room temperature for 2 h. The reaction mixture was concentrated under reduced pressure to give after purification by preparative HPLC Example 24 as a white solid. Yield (200 mg, 50%); 1H NMR (400 MHz, DMSO-d6) δ 8.39 (s, 1H), 8.31 (d, J=7.6 Hz, 1H), 8.20 (d, J=7.6 Hz, 1H), 7.88 (m, 4H), 3.56-3.52 (m, 2H), 3.50-3.47 (m, 2H), 3.20-3.17 (m, 4H), 3.05-3.02 (m, 2H), 2.31 (bs, 1H), 2.17-2.14 (m, 2H), 1.85-1.77 (m, 2H); MS: m/z 360.18 [M+H]+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09133154B2 |
| Source dataset | uspto-grants-2015_09 |
| ORD ID | ord-ac4cc71e5307449cb5064c804f4dc9e5 |
| Source note | uspto-grants-2015_09 |