HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethyl bromoacetate → HCID 22321977, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethyl bromoacetate | HCID 7748 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | 2,6-Dichloro-4-hydroxymethylbenzaldehyde | HCID 10242032 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 22321977 | HCID 22321977 | — |
Reaction Conditions
| Temperature | 110 °C |
|---|
Reaction Steps
A solution of 500 mg (2.4 mmol) A3 in 5 ml dry dimethyl formamide under nitrogen was cooled in an ice bath and 73 mg (3.0 mmol) sodium hydride was added and the mixture was stirred for 10 minutes. After addition of 410 mg (2.6 mmol) ethyl bromoacetate, the mixture was heated to 110° C. for 8 h. The solvent was removed in vacuo and the residue was taken up in ethyl acetate and washed with water. The organic layer was dried over sodium sulphate and evaporated to dryness. Purification of the residue by column chromatography on SiGel (heptane/ethyl acetate 4:1) yielded 40 mg (6%) A15.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06790852B2 |
| Source dataset | uspto-grants-2004_09 |
| ORD ID | ord-9bcd876289e043a89f22f75f54b81fb6 |
| Source note | uspto-grants-2004_09 |