HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethyl bromoacetate → 4-ethoxycarbonylmethyl-7-nitro-2H-1,4-benzoxazin-3(4H)-one
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethyl bromoacetate | HCID 7748 | — |
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | 7-nitro-3,4-dihydro-2H-1,4-benzoxazin-3-one | HCID 2763830 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | 4-ethoxycarbonylmethyl-7-nitro-2H-1,4-benzoxazin-3(4H)-one | HCID 11150183 | 71.4% |
Reaction Steps
Ethyl bromoacetate (18.4 g) was added dropwise at a temperature of 30° C. to 40° C. to a mixture of 7-nitro-2H-1,4-benzoxazin-3(4H)-one (19.4 g), potassium carbonate (15.2 g) and acetonitrile (100 ml), the mixture was refluxed under heating for 3 hours. When the reaction was completed, the liquor was filtered, the filtrate was distilled. Recrystallization of the resulting solid from toluene-hexane gave the desired 4-ethoxycarbonylmethyl-7-nitro-2H-1,4-benzoxazin-3(4H)-one (20 g). mp. 120.5°-121.5° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04798620 |
| Source dataset | uspto-grants-1989_01 |
| ORD ID | ord-59bbc318485c499daee91d5f32eef94f |
| Source note | uspto-grants-1989_01 |