HuagongsheHuagongshe Chemistry Print Report · For research reference only
Benzene → HCID 62397384, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Benzene | HCID 241 | — |
| Reactant | Ethanol | HCID 702 | — |
| Reactant | HCID 57474515 | HCID 57474515 | — |
| Catalyst | p-Toluenesulfonic acid monohydrate | HCID 521998 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 62397384 | HCID 62397384 | 85% |
Reaction Steps
To a mixture of 25.0 g of Intermediate 1 (Example 1), 20 g of ethanol and 200 g of benzene was added 0.15 g of p-toluenesulfonic acid monohydrate. With stirring in a nitrogen atmosphere, the mixture was heated for 20 hours while water of reaction was sequentially removed out of the system. After cooling, the reaction mixture was poured into a saturated sodium hydrogen carbonate aqueous solution and extracted with ethyl acetate. The ethyl acetate solution was washed, dried, and concentrated, obtaining 24.5 g (yield 85%) of crude ethyl 2,2-difluoro-3-hydroxy-5-methylhexanoate. This crude product had a sufficient purity as an intermediate and was ready for use in the subsequent step.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09261783B2 |
| Source dataset | uspto-grants-2016_02 |
| ORD ID | ord-dea65e2c2153492fa2f4474d263e8b98 |
| Source note | uspto-grants-2016_02 |