HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetic Acid → Dimethyl 2-Oxo-3-methylheptylphosphonate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetic Acid | HCID 176 | — |
| Reactant | Tetrahydrofuran | HCID 8028 | — |
| Reactant | Dimethyl methylphosphonate | HCID 12958 | — |
| Reactant | Butyllithium | HCID 178418339 | — |
| Product | Dimethyl 2-Oxo-3-methylheptylphosphonate | HCID 12906670 | — |
Reaction Steps
To a THF (120 ml) solution of dimethyl methylphosphonate (5.04 g) at -60° C. was added dropwise n-BuLi (1.6-M, 25.4 ml), and the mixture was stirred for 30 min. A THF (50 ml) solution of methyl 2R,S-methylcaproate (3 15 g) was added dropwise. The mixture was stirred at -60° C. for 1 h, then at room temperature for 1.5 h, and thereafter acetic acid (2 ml) was added at 0° C. A crude product obtained after the usual work-up was chromatographed (hexane : ethyl acetate=1 : 5). Yield : 2,85 g (58%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05166174 |
| Source dataset | uspto-grants-1992_11 |
| ORD ID | ord-55ad27566e2d406cae1d0bc2d573e2df |
| Source note | uspto-grants-1992_11 |