Methyl chloroformate → Methyl 2-(trifluoromethoxy)phenyl carbonate

Temperatur

0 °C

2-(Trifluoromethoxy)phenol (6.0 g, 32.7 mmol) was dissolved in methylene chloride and triethylamine (9.1 mL, 65.4 mmol). The mixture was cooled to 0° C. and methyl chloroformate (2.8 mL, 36.0 mmol) was added dropwise. The mixture was stirred for 2 h at room temperature then quenched with saturated NH4Cl. The reaction was diluted with water and the aqueous layer extracted with dichloromethane (2×30 mL). The combined extracts were washed with water (100 mL) and brine (100 mL), dried over MgSO4, filtered and concentrated in vacuo to provide methyl 2-(trifluoromethoxy)phenyl carbonate (7.1 g, 92% yield). 1H NMR (400.0 MHz, DMSO-d6) δ7.36-7.26 (m, 4H), 3.93 (s, 3H).

1. customthen quenched with saturated NH4Cl
2. additionThe reaction was diluted with water
3. extractionthe aqueous layer extracted with dichloromethane (2×30 mL)
4. washThe combined extracts were washed with water (100 mL) and brine (100 mL)
5. dry with materialdried over MgSO4
6. filtrationfiltered
7. concentrationconcentrated in vacuo

ORD-Eintrag

ord-700cfeb0cd194b2699109474c673a4f7

Quelldatensatz

uspto-grants-2014_01

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US08633189B2