Sodium Hydroxide → 2-Amino-3-chlorophenol

Temperatur

80 °C

A mixture of 3-chloro-2-nitrophenol(250 mg, 1.4 mmol) and tin (II) chloride (1.2 g, 5.3 mmol) in ethanol(50 mL) was heated at 80° C. under argon. After 2 hours, the starting material has disappeared and the solution was allowed to cool down and then poured into ice. The pH was made slightly basic (pH7-8), by addition of solid NaOH, before being extracted with ethyl acetate. The organic phase was washed with brine, dried over MgSO4 and filtered. The solvent was evaporated and chromatography of the resulting solid on silica gel (4%MeOH/CH2 Cl2) gave the desired product(143 mg, 69%). 1H NMR (CD3 OD): d 6.75 (t,1H), 6.70 (d, 1H), 6.65 (d, 1H).

1. temperatureto cool down
2. additionpoured into ice
3. extractionbefore being extracted with ethyl acetate
4. washThe organic phase was washed with brine
5. dry with materialdried over MgSO4
6. filtrationfiltered
7. customThe solvent was evaporated

ORD-Eintrag

ord-9d304334c07e407caa880a618cffb648

Quelldatensatz

uspto-grants-1998_07

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US05780483