Methyl formate → HCID 86666219, Verbindung

To a suspension of NaH (0.512 g, 12.81 mmol) in DME (15 mL) was added a solution of methyl 4,4,4-trifluorobutanoate (1 g, 6.41 mmol) and methyl formate (0.594 mL, 9.61 mmol) in DME (10 mL) dropwise at 0° C. The mixture was stirred at room temperature overnight. After removing the solvent, the residue was diluted with water (50 mL), extracted with ether once, and neutralized to pH<7 by AcOH. The aqueous layer was separated and extracted with EA twice. The combined organic phase was dried over sodium sulfate, filtered, and concentrated to afford the title compound (0.875 g, 4.75 mmol, 74.2% yield). LCMS: rt=2.23 min, [M+H+]=185

1. customAfter removing the solvent
2. additionthe residue was diluted with water (50 mL)
3. extractionextracted with ether once
4. customThe aqueous layer was separated
5. extractionextracted with EA twice
6. dry with materialThe combined organic phase was dried over sodium sulfate
7. filtrationfiltered
8. concentrationconcentrated

ORD-Eintrag

ord-5dc5507b6fc44d6aace00df2603b5236

Quelldatensatz

uspto-grants-2014_01

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US08637536B2