Hexane → HCID 86732218, Verbindung

To a cooled (−78° C.) solution of 1,2-difluorobenzene (8.81 mL, 89 mmol) in THF (175 mL) was added dropwise butyllithium solution, 1.6M in hexane (61.5 mL, 98 mmol). After stirred for 2 h, ethyl fluoroacetate (8.64 mL, 89 mmol) ethyl fluoroacetate was added dropwise. The reaction was stirred for 1 h, the reaction was quenched with saturated NH4Cl and then warmed to room temperature. The resulted mixture was extracted with EtOAc. The organic extracts were washed with brine, dried over Na2SO4 and filtered. The filtrate was concentrated and purified by silica gel column (0-30% EtOAc/hexane) to afford 6.3 g of desired product as colorless oil.

1. stirringThe reaction was stirred for 1 h
2. customthe reaction was quenched with saturated NH4Cl
3. extractionThe resulted mixture was extracted with EtOAc
4. washThe organic extracts were washed with brine
5. dry with materialdried over Na2SO4
6. filtrationfiltered
7. concentrationThe filtrate was concentrated
8. custompurified by silica gel column (0-30% EtOAc/hexane)

ORD-Eintrag

ord-9212a8e4f02a4fcabb651f686eb4ea5a

Quelldatensatz

uspto-grants-2016_03

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US09296734B2