HuagongsheHuagongshe Chemistry Print Report · For research reference only
1,8-Diazabicyclo(5.4.0)undec-7-ene → HCID 86701169, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1,8-Diazabicyclo(5.4.0)undec-7-ene | HCID 81184 | — |
| Reactant | PyBOP | HCID 2724699 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | HCID 86701169 | HCID 86701169 | 136.7% |
Reaction Steps
A mixture of this material (10 g, 68.0 mmol) and PyBOP (38.9 g, 74.8 mmol) in acetonitrile (250 mL) was treated with DBU (12.2 mL, 81.6 mmol) and stirred for 2.5 h. The reaction mixture was filtered, and the precipitate was washed with diethyl ether (3×50 mL) and dried under vacuum. The title compound (13.51 g, 75%) was obtained as a cream-coloured solid. δH (DMSO-d6) 9.28 (dd, J 4.2, 1.6 Hz, 1H), 8.82 (s, 1H), 8.59 (dd, J 8.6, 1.5 Hz, 1H), 8.24-8.18 (m, 2H), 7.88-7.85 (m, 1H), 7.69-7.64 (m, 1H), 7.60-7.54 (m, 1H). LCMS (ES+) 265 (M+H)+, RT 1.23 minutes.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09029392B2 |
| Source dataset | uspto-grants-2015_05 |
| ORD ID | ord-2d865ec4ef634390b51ef488f41aa3ac |
| Source note | uspto-grants-2015_05 |