HuagongsheHuagongshe Chemistry Print Report · For research reference only
Bromine → 5-Bromo-3-ethyl-1,3-dihydro-indol-2-one
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Bromine | HCID 24408 | — |
| Reactant | 3-Ethylindolin-2-one | HCID 347325 | — |
| Reactant | Sodium Acetate | HCID 517045 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Solvent | Water | HCID 962 | — |
| Product | 5-Bromo-3-ethyl-1,3-dihydro-indol-2-one | HCID 2771852 | — |
Reaction Steps
A solution of 3-ethyloxindole (6.0 g, 40 mmol) and sodium acetate (4 g, 48 mmol) in acetic acid (100 ml) was treated with bromine (6.4 g, 40 mmol). After 30 min. the mixture was diluted with water and extracted with EtOAc (2×); the combined organic layers were washed with water, sat. sodium hydrogen carbonate solution, and brine, dried (MgSO4) and evaporated to afford the crude product (9.2 g, 96%). A sample was recrystallized from EtOAc/hexane to obtain the subtitled compound, m.p. 130-132° C.; 1H-NMR (DMSO-d6) δ 0.74 (t, 3H, J=7.5 Hz), 1.8-2.0 (m, 2H), 3.45 (t, 1H, J=5.5 Hz,), 6.76 (d, 1H, J=8.35 Hz), 7.42 (m, 1H), 10.43 (s, 1H); MS (−ESI) m/z 238/240 (M−H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06608068B2 |
| Source dataset | uspto-grants-2003_08 |
| ORD ID | ord-a44d07ae1abf4de7919c6ba98d660275 |
| Source note | uspto-grants-2003_08 |