Methyl formate → HCID 86666219, 화합물

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 기록

ord-d567824221594860bf96c3bd7cbf30f0

출처 데이터셋

uspto-grants-2015_11

DOI

10.6084/m9.figshare.5104873.v1

특허 번호

US09174968B2