HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → HCID 86709261, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Ethyl Acetate | HCID 8857 | — |
| Reactant | (Diethoxyphosphoryl)acetyl chloride | HCID 10822542 | — |
| Reactant | HCID 86709262 | HCID 86709262 | — |
| Product | HCID 86709261 | HCID 86709261 | 42% |
Reaction Steps
2.0 g (13.51 mmol) of 2-hydroxyethylmethyl oxalate and 1.7 g (16.8 mmol) of triethylamine were dissolved in 50 mL of ethyl acetate, and 3.1 g (14.5 mmol) of diethyl (2-chloro-2-oxoethyl)phosphonate was dropwise added thereto at 15° C. or lower, taking 15 minutes. This was stirred at room temperature for 1 hour, and the disappearance of the starting materials was confirmed through gas chromatography. The reaction liquid was washed with water, the organic layer was concentrated under reduced pressure, and the resulting residue was purified through silica gel column chromatography (ethyl acetate for elution) to give 1.8 g (yield 42%) of the intended 2-(2-(diethoxyphosphoryl)acetoxyl)ethyl methyl oxalate.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09384906B2 |
| Source dataset | uspto-grants-2016_07 |
| ORD ID | ord-bc11775d59194849bf58191c739ae67b |
| Source note | uspto-grants-2016_07 |