HuagongsheHuagongshe Chemistry Print Report · For research reference only
Benzene → HCID 86663804, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Benzene | HCID 241 | — |
| Reactant | 2-Methoxyethanol | HCID 8019 | — |
| Reactant | HCID 57474515 | HCID 57474515 | — |
| Catalyst | p-Toluenesulfonic acid monohydrate | HCID 521998 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 86663804 | HCID 86663804 | 73% |
Reaction Steps
To a mixture of 25.0 g of Intermediate 1 (Example 1), 25 g of 2-methoxyethanol 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 8 hours while water of reaction was sequentially removed out of the system. After cooling, the reaction mixture was poured into ice water and extracted with ether. The ether solution was washed, dried, and concentrated, obtaining 23.9 g (yield 73%) of crude 2-methoxyethyl 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-8feb188f7c8e4ce981dd446704819ea1 |
| Source note | uspto-grants-2016_02 |