HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 10998727, compound → HCID 10857224, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 10998727 | HCID 10998727 | — |
| Reactant | HCID 178418361 | HCID 178418361 | — |
| Solvent | Isopropanol | HCID 3776 | — |
| Product | HCID 10857224 | HCID 10857224 | 98.6% |
Reaction Steps
In a 200 ml Hastelloy autoclave was put 50 g (GC p=93.2%, 220 mmol) of methyl 4-phenyl-2-chloro-3-oxobutyrate (compound (III)), 99.4 mg (0.055 mmol) of Ru2Cl4 [(R)-T-BINAP]2NEt3, and 100 ml of isopropyl alcohol (IPA) under a nitrogen stream. After heating the solution, a hydrogen pressure of 30 atm was introduced into the autoclave at 100° C. to initiate the reaction. Then, it was confirmed by GC that no unreacted matter remained to complete the reaction (for 1 to 2 hours). IPA was recovered under reduced pressure at not higher than 50° C. to obtain 50.3 g [GC p=92.2%, HPLC o.p. syn 87% (80.5% ee), anti 13% (94.6% ee)] of compound (IV) in a yield of 98.6%.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05581007 |
| Source dataset | uspto-grants-1996_12 |
| ORD ID | ord-3f79d7daa95d4411a65329864eb5cd88 |
| Source note | uspto-grants-1996_12 |