HuagongsheHuagongshe Chemistry Print Report · For research reference only
4-Bromophenacyl bromide → HCID 59822262, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 4-Bromophenacyl bromide | HCID 7454 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | N-Cyclopropylmethylthiourea | HCID 2795339 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 59822262 | HCID 59822262 | 91% |
Reaction Steps
Slurry 4-bromophenacyl bromide (11.2 g, 50 mmol) in absolute ethanol (50 mL). Add N-cyclopropylmethyl-thiourea (6.5 g, 50 mmol) and sodium bicarbonate (4.2 g, 50 mmol), heat to reflux for 2 h, then stir at room temperature overnight. Concentrate to ¼ volume and partition between water/EtOAc (4:1, 500 mL). Extract the aqueous layer with EtOAc (2×75 mL). Dry the combined organic extracts over Na2SO4, filter and concentrate in vacuo to obtain the title compound (14.0 g, 91%) as an off-white solid that was used without further purification. MS (ES+) m/z: 310 (M+H)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07994163B2 |
| Source dataset | uspto-grants-2011_08 |
| ORD ID | ord-7a818e54f2c74bdb9d0979692aa8fdcb |
| Source note | uspto-grants-2011_08 |