Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Dimethylformamide | HCID 6228 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | Phosphorus oxychloride | HCID 24813 | — |
| Reactant | methyl 2-amino-4,5-diethoxybenzoate | HCID 3516698 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 22466704 | HCID 22466704 | — |
Reaction Steps
To a stirred solution of methyl 2-amino-4,5-diethoxybenzoate (4.79 g, 20 mmol) in 20 ml of DMF at 0° C. was added phosphorous oxychloride (2.24 ml, 24 mmol) during 15 m. The mixture was warmed to 55° C. and stirred for 45 m. The resulting solution was diluted with methylene chloride, cooled to 0° C., and treated with 80 ml of precooled N/1 sodium hydroxide during 5 m. The organic layer was separated and washed at 0° C. with with water. The solution was dried and concentrated to give an amber oil; NMR (CDCl3) δ3.00(s, Me2N).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US06288082B1 |
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| Source dataset | uspto-grants-2001_09 |
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| ORD ID | ord-d3c2fe74ead4432e988badee03fdd6d3 |
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| Source note | uspto-grants-2001_09 |
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