HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethyl bromoacetate → HCID 11234214, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethyl bromoacetate | HCID 7748 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | Methyl 3-hydroxy-2-(4-methoxybenzenesulfonylamino)propionate | HCID 11173760 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 11234214 | HCID 11234214 | 72% |
Reaction Steps
The compound of Example 1 (5.65 g, 19.5 mmol) and anhydrous potassium carbonate anhydrous (8 g, 60 mmol) were suspended in DMF (35 mL), a catalytic amount of Et3N was introduced, and ethyl bromoacetate (4.3 mL, 40 mmol) was added dropwise. After stirring for 5 hours, 50 mL of distilled water and 100 mL of ethyl acetate were introduced and stirred to separate layers. The supernatant was washed with a 1N HCl aqueous solution (50 mL), a saturated NaHCO3 aqueous solution (50 mL), and distilled water (100 mL), and it was dried and concentrated under reduced pressure. The mixture was separated using hexane and ethylacetate (2:1) in a silica gel column to obtain a yellow thick oily title compound (5.26 g, yield 72%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07223751B2 |
| Source dataset | uspto-grants-2007_05 |
| ORD ID | ord-b2997a760b5b487db3dcc23887b60db2 |
| Source note | uspto-grants-2007_05 |