HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dimethyl diethylmalonate → Bis-(1-allyl-2,2,6,6-tetramethyl-4-piperidinyl) diethylmalonate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dimethyl diethylmalonate | HCID 117935 | — |
| Reactant | 2,2,6,6-Tetramethyl-1-(prop-2-en-1-yl)piperidin-4-ol | HCID 12991975 | — |
| Solvent | O-Xylene | HCID 7237 | — |
| Product | Bis-(1-allyl-2,2,6,6-tetramethyl-4-piperidinyl) diethylmalonate | HCID 20512150 | — |
Reaction Steps
After the addition of 1 g of tetrabutyl-orthotitanate, 47 g of dimethyl diethylmalonate and 98.6 g of 1-allyl-2,2,6,6-tetramethyl-4-hydroxypiperidine in 100 ml of xylene are heated under a gentle stream of nitrogen to about 140°. The methanol forming during the reaction is continuously distilled off, and after about 6 hours the reaction is virtually completed. The reaction mixture is diluted with 200 ml of toluene, extracted three times with 100 ml of water each time, dried over sodium sulphate and concentrated by evaporation. Crystallisation of the residue from hexane yields bis-(1-allyl-2,2,6,6-tetramethyl-4-piperidinyl) diethylmalonate (compound 18), m.p. 135°-136°.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04293468 |
| Source dataset | uspto-grants-1981_10 |
| ORD ID | ord-9880888cada64eb0b2423ff6cef9425a |
| Source note | uspto-grants-1981_10 |