HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 67236755, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Diethyl Ether | HCID 3283 | — |
| Reactant | HCID 131731307 | HCID 131731307 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 67236755 | HCID 67236755 | 84% |
Reaction Steps
A solution of 4 N hydrogen chloride in dioxane (8 mL) was treated with the compound of Example 70B (136 mg, 0.21 mmol) followed by stirring at RT for 2 h. (During this time, the mono-deprotection product started precipitating, and ca. 4 mL of dichloromethane was added to speed the reaction by solublizing the mono-hydrochloride) The mixture was added to excess ether and the product collected by filtration and washed with ether. After drying in a vacuum oven at 50° C. for 18 h, these procedures afforded the title compound (92 mg, 84%) as an off-white powder. 1H NMR (400 MHz, DMSO-d6) δ 7.28 (m, 8 H), 6.81 (t, J=8.9 Hz, 2 H), 6.33 (m, 2 H), 5.63 (m, 2 H), 5.51 (dd, J=5.5, 1.9 Hz, 2 H), 1.79 (s, 6 H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08691938B2 |
| Source dataset | uspto-grants-2014_04 |
| ORD ID | ord-840a618d71394983a45be6a23570569e |
| Source note | uspto-grants-2014_04 |