2,2,2-Trifluoroethanol → HCID 19381016, Verbindung

To a mixture of sodium hydride (1.648 g, 68.66 mmol) in tetrahydrofuran (220 mL) at 0° C. was added 2,2,2-trifluoroethanol (5.0 mL, 68.66 mmol). After 5 minutes, the reaction was allowed to warm to room temperature and methyl 2-bromoacetate (6.2 mL, 65.39 mmol) was added. After stirring for 72 hours, the mixture was filtered through diatomaceous earth with ether washes. The filtrate was concentrated and distilled to afford the title compound as a colorless oil (8.26 g, 73%), bp 155°-60° C., MS(CI): 173(M+H); H-NMR (300 MHz, DMSO-d6): 3.68(s, 3H), 4.16(q, J=9.2 Hz, 2H), 4.33(s, 2H).

1. filtrationthe mixture was filtered through diatomaceous earth with ether washes
2. concentrationThe filtrate was concentrated
3. distillationdistilled

ORD-Eintrag

ord-1b4e6061c4db43b484a943601731d4b0

Quelldatensatz

uspto-grants-1993_11

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US05266570