* All experimental methods are cited from the reference, please refer to the original source for details. We do not guarantee the accuracy of the content in the reference.
b) Preparation of 2-amino-5,6 dichlorophenol A mixture of 5,6-dichloro-2-nitrophenol(1.8 g, 8.7 mmol) and tin (II) chloride (5.8 g, 26.1 mmol) in ethanol(50 mL) was heated at 80 C. under argon. After 2 hours, the starting material had 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(1.4 mg, 90%). 1 H NMR (CD3 OD): delta 6.71 (d, 1H), 6.45 (d, 1H).
90%
In ethanol;
b)Preparation of 2-amino-5,6 dichlorophenol A mixture of 5,6-dichloro-2-nitrophenol(1.8 g, 8.7 mmol) and tin (II) chloride (5.8 g, 26.1 mmol) in ethanol(50 mL) was heated at 80-- C under argon. After 2 hours, the starting material had 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(1.4 mg, 90%). 1 H NMR (CD3 OD): d 6.71 (d, 1H), 6.45 (d, 1H).
90%
In ethanol;
b) Preparation of 2-amino-5,6 dichlorophenol A mixture of 5,6-dichloro-2-nitrophenol (1.8 g, 8.7 mmol) and tin (II) chloride (5.8 g, 26.1 mmol) in ethanol (50 mL) was heated at 80 C. under argon. After 2 hours, the starting material had 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/CH2CH2) gave the desired product (1.4 mg, 90%). 1H NMR (CD3OD): d 6.71 (d, 1H), 6.45 (d, 1H).
90%
In ethanol;
b)Preparation of 2-amino-5,6 dichlorophenol A mixture of 5,6-dichloro-2-nitrophenol(1.8 g, 8.7 mmol) and tin (II) chloride (5.8 g, 26.1 mmol) in ethanol(50 ml) was heated at 80 C. under argon. After 2 hours, the starting material had 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/CH2Cl2) gave the desired product(1.4 mg, 90%). 1H NMR (CD3OD): delta6.71 (d, 1H), 6.45 (d, 1H).
tert-butyl (3,4-dichloro-2-hydroxyphenyl)carbamate[ No CAS ]
Yield
Reaction Conditions
Operation in experiment
74%
With zinc(II) chloride; In dichloromethane;
To a solution of <strong>[116278-69-4]6-amino-2,3-dichlorophenol</strong> (100 mg, 0.57 mmol) in DCM (5 mL) were added Boc2O (370 mg (1.7 mmol) and ZnCl2 (77 mg, 0.57 mmol). The reaction mixture was stirred overnight, diluted with EA and washed with H2O and brine. The organic layer was collected, dried (Na2SO4), filtered and concentrated. The residue was purified by chromatography (EA/ Hexanes) to provide 116 mg (74%) of Intermediate 43A. LCMS [m/z] calculated for C11H13Cl2NO3: 277.0 found 278.2 [M+H]+, tR=5.33 min (Method 4).
Chemistry
Pharmaceutical Intermediates
Inhibitors/Agonists
Material Science
For Research Only
110K+ Compounds
Competitive Price
1-2 Day Shipping
