HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanol → HCID 86663801, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | HCID 57474515 | HCID 57474515 | — |
| Catalyst | p-Toluenesulfonic acid monohydrate | HCID 521998 | — |
| Product | HCID 86663801 | HCID 86663801 | 72% |
Reaction Steps
To a mixture of 28.11 g of Intermediate 1 (Example 1) and 280 g of methanol was added 0.6 g of p-toluenesulfonic acid monohydrate. With stirring in a nitrogen atmosphere, the mixture was heated under reflux for 8 hours. After cooling, the reaction mixture was concentrated to about 200 ml. The concentrate was poured into a saturated sodium hydrogen carbonate aqueous solution and extracted with ether. The ether solution was washed, dried, and concentrated, obtaining 21.8 g (yield 72%) of methyl 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 | US08697903B2 |
| Source dataset | uspto-grants-2014_04 |
| ORD ID | ord-18d3a8929f07489ab962858cb67332c2 |
| Source note | uspto-grants-2014_04 |