HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethyl Acetate → HCID 86650255, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethyl Acetate | HCID 8857 | — |
| Reactant | Phosphorus sulfide (P2S5) | HCID 14817 | — |
| Reactant | 5-(3-Bromophenyl)-5-(difluoromethyl)-3-morpholinone | HCID 66665407 | — |
| Solvent | Pyridine | HCID 1049 | — |
| Product | HCID 86650255 | HCID 86650255 | — |
Reaction Steps
5-(3-Bromo-phenyl)-5-difluoromethyl-morpholin-3-one (6.10 g, 19.93 mmol) was dissolved in 63 ml dry pyridine, and P2S5 (5.32 g, 23.91 mmol) was added. The mixture was heated to 80° V for 2 hrs. After completion, the mixture was put between ethyl acetate and 1 H HCl solution. Phases were separated and the organic phase was washed with 1 N HCl, saturated NaHCO3 solution and brine. The organic phases were combined, dried over Na2SO4 and concentrated under reduced pressure to yield the title compound as off-white solid. 1H-NMR (360 MHz, DMSO-d6): 8.60 (s, 1H, NH), 7.80-7.35 (m, 4H), 6.54 (t, 1H, CHF2), 4.45 (m, 2H), 4.28 (d, 1H), 4.12 (d, 1H); MS: 322 [(M+H)+].
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08846658B2 |
| Source dataset | uspto-grants-2014_09 |
| ORD ID | ord-23cee72225db41cc8abc246ce8820549 |
| Source note | uspto-grants-2014_09 |