HuagongsheHuagongshe Chemistry Print Report · For research reference only
Bromine → HCID 59277594, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Bromine | HCID 24408 | — |
| Reactant | HCID 59277595 | HCID 59277595 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Product | HCID 59277594 | HCID 59277594 | 71% |
Reaction Steps
Bromine (43 ul, 0.84 mmol) was added drop wise to a solution of (S)-2-methyl-1,2,4,5-tetrahydropyrido[2,3-e][1,4]diazepin-3-one (136 mg, 0.77 mmol) in acetic acid (10 mL). The reaction was stirred at room temperature for 3 h. The reaction was quenched with sat. NaHCO3 (10 mL) and extracted with ethyl acetate (3×15 mL), dried over sodium sulfate and concentrated to give the title compound (140 mg, 71%): 1H NMR (400 MHz, CDCl3) δ 7.93 (s, 1H), 7.31 (s, 1H), 7.20 (b, 1H), 5.95 (bs, 1H), 4.97-4.91 (m, 1H), 4.72-4.70 (m, 1H), 3.85-3.79 (m, 1H), 1.47 (d, J=6.4 Hz, 3H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08450307B2 |
| Source dataset | uspto-grants-2013_05 |
| ORD ID | ord-75581c2442354f2681b865712650e9b8 |
| Source note | uspto-grants-2013_05 |