HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 239549, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | 3-Chloro-1,2-propanediol | HCID 7290 | — |
| Reactant | Ethyl Acetoacetate | HCID 8868 | — |
| Catalyst | p-Toluenesulfonic acid | HCID 6101 | — |
| Solvent | Hexane | HCID 8058 | — |
| Product | HCID 239549 | HCID 239549 | 72% |
Reaction Steps
In a similar manner to the preceding Examples, 65 g (0.5 mol) of ethyl acetoacetate are heated together with 55 g (0.5 mol) of 3-chloro-1,2-propanediol and 0.2 g of p-TSA in a water separator. 100 ml of hexane act as entraining agent. Once 9 ml of water have separated, the reaction mixture is washed with 100 ml of water, to which 1 g of NaOH is added, dried over Na2SO4 and fractionated. 80 g (72%) of 2-methyl-2-ethoxycarbonylmethyl-4-chloromethyl-1,3-dioxolane are obtained. Bp.: 124° C. (1500 Pa); IR: 1736 cm−1 (C═O, ester); MS: m/e=207 (M−15), 181, 173, 157, 144, 135, 115, 99, 75, 57, 43.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06388104B1 |
| Source dataset | uspto-grants-2002_05 |
| ORD ID | ord-da2b8564fa5c40499e6b0ab580a75d18 |
| Source note | uspto-grants-2002_05 |