HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 178478956, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | HCID 178506071 | HCID 178506071 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 178478956 | HCID 178478956 | 90% |
Reaction Steps
3-[5-(2-Chloro-phenyl)-7-trifluoromethyl-1H-benzimidazol-2-yl]-1-oxa-2-aza-spiro[4.5]dec-2-ene (1.14 g, 2.63 mmol, as prepared in the previous step) was placed in a 100 mL round-bottom flask, and EtOAc (10 mL) was added. HCl (1 eq., 2.60 mL, 2.63 mmol, 1 M solution in ether) was added via syringe. The solvent was removed under reduced pressure, and the solid was dried under high vacuum for 3 days, yielding 1.12 g (90%) of the desired compound. 1H-NMR (400 MHz, d6-DMSO) δ: 7.80 (s, 1H), 7.60-7.66 (m, 1H), 7.59 (s, 1H), 7.52-7.58 (m, 1H), 7.43-7.51 (m, 2H), 1.61-1.82 (m, 6H), 1.32-1.59 (m, 4H). Mass Spectrum (LCMS, ESI pos.): Calcd. for C22H19ClF3N3O: 434.1 (M+H). found: 434.2.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08232409B2 |
| Source dataset | uspto-grants-2012_07 |
| ORD ID | ord-c072796e4654432eaf5d9ebcbcf621ff |
| Source note | uspto-grants-2012_07 |