HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → HCID 19938496, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | 1,3,2-Dioxaphosphorinane, 2-chloro-5,5-dimethyl- | HCID 75508 | — |
| Reactant | HCID 10541232 | HCID 10541232 | — |
| Solvent | Mesitylene | HCID 7947 | — |
| Product | HCID 19938496 | HCID 19938496 | 57.1% |
Reaction Steps
4.85 g (29.0 mmol) of 2-chloro-5,5-dimethyl-1,3,2-dioxaphosphorinane are added drop-wise over a period of about 15 minutes to a solution of 6.6 g (27.0 mmol) of 6-(cyclohexen-1-yl)-2-tert-butyl-4-methylphenol (compound (102), Example 1) and 4.0 ml (29.0 mmol) of triethylamine in 25 ml of mesitylene (1,3,5-trimethylbenzene). The reaction mixture is then refluxed for 18 hours, cooled, filtered, and the filtrate is concentrated on a vacuum rotary evaporator. Crystallization of the residue from dry acetonitrile gives 5.8 g (57%) of 2-[6-(cyclohexen-1-yl)-2-tert-butyl-4-methyl-phenoxy]-5,5-dimethyl-1,3,2-dioxaphosphorinane, m.p. 97°-102° C. (compound (201), Table 2).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05414033 |
| Source dataset | uspto-grants-1995_05 |
| ORD ID | ord-3eb776d53dbb47d187b3886d19165e6e |
| Source note | uspto-grants-1995_05 |