Methanol → HCID 12933608, compound

In a 500 ml flask were charged 300 ml of methanol, 35.5 g of (R)-3-methylheptanoic acid obtained in Step 3, and 0.5 g of concentrated sulfuric acid, and the mixture was heated at a methanol refluxing temperature for 18 hours. Methanol was distilled off under reduced pressure, and the residue was extracted with diethyl ether. The extract was washed with water, neutralized with a sodium carbonate aqueous solution, and then washed with a sodium chloride aqueous solution. Diethyl ether was removed by distillation, and the residue was distilled under reduced pressure to obtain 29 g (76.8%) of the titled compound (b.p.: 80° C./20 mmHg).

1. distillationMethanol was distilled off under reduced pressure
2. extractionthe residue was extracted with diethyl ether
3. washThe extract was washed with water
4. washwashed with a sodium chloride aqueous solution
5. customDiethyl ether was removed by distillation
6. distillationthe residue was distilled under reduced pressure

ORD record

ord-1e71757b4d5c4c878294376af74fbfe6

Source dataset

uspto-grants-2000_07

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US06093345