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CAS No. : | 22996-18-5 | MDL No. : | MFCD00007217 |
Formula : | C7H6ClNO3 | Boiling Point : | No data available |
Linear Structure Formula : | - | InChI Key : | OAHGNOHGHOTZQU-UHFFFAOYSA-N |
M.W : | 187.58 | Pubchem ID : | 89956 |
Synonyms : |
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Signal Word: | Warning | Class: | |
Precautionary Statements: | P261-P305+P351+P338 | UN#: | |
Hazard Statements: | H315-H319-H335 | Packing Group: | |
GHS Pictogram: |
* 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.
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
97% | With iron; ammonium chloride; In ethanol; water; for 2h;Reflux; | General procedure: Iron powder (5.5 eq.) and NH4Cl (0.7 eq.) were suspended in EtOH : H2O 10 : 1 (0.05 M) and refluxedwith nitrophenyl derivative 12 (1 eq.) for 2 h. After completion (monitored by TLC analysis), thereaction mixture was filtrated on Celite and rinsed with CH2Cl2. The solvent was evaporated underreduced pressure and CH2Cl2 was added. The mixture was washed with a saturated solution ofNaHCO3. The aqueous phase was extracted four times with CH2Cl2 and the combined organic phaseswere washed with brine, dried over magnesium sulfate and filtrated. Evaporation of the solvent underreduced pressure gave the desired product 11, which was used in the next step without furtherpurification. |
77% | With hydrogen;platinum(IV) oxide; In ethanol; at 20℃; under 975.0980000000001 Torr; for 1h; | A suspension of (4-chloro-2-nitrophenyl)methanol (1 g, 5.33 mmol, ALDRICH) and platinum(IV) oxide (100 mg, 0.44 mmol) in ethanol (100 mL) was hydrogenated under 1300 mbar at room temperature for 1 hour. The resulting suspension was filtered, washed with ethanol and the filtrate concentrated to dryness to afford the crude (2-amino-4- chlorophenyl) methanol as a pale orange solid. The crude product was purified by flash <n="180"/>chromatography on silica gel eluting with 0 to 3% methanol in dichloromethane. The solvent was evaporated to dryness to afford (2-amino-4-chlorophenyl)methanol (0.650 g, 77 %) as a pale orange solid. NMR Spectrum (DMSOdthetaV. 4.34 (d, 2H), 5.06 (t, IH), 5.20 (s, 2H), 6.51 (dd, IH), 6.64 (d,IH), 7.05 (d, IH) |
With hydrogen;5% platinum on sulfided carbon; In ethanol; for 2h; | (4-chloro-2-nitrophenyl)methanol (40.0 g, 0.21 mol) was dissolved in ethanol (700 ml_) and hydrogenated under hydrogen gas (20 psi) in the presence of 5% platinum on sulfided carbon (Pt-C/S) (5.0Og). After 2 hours the catalyst was removed by filtration through Celiteand the solvent removed under reduced pressure. This provided the desired compound (2-amino-4-chlorophenyl)methanol (32.9 g) which was used without further purification. HPLC Rt =1.70 minutes. 1H NMR (CDCI3) delta 6.96 (d, 1 H), 6.67 (m, 2H), 4.64 (s, 2H), 4.27 (bs, 2H)1 1.56 (bs, 1 H). |
32.9 g | With hydrogen; In ethanol; under 1034.32 Torr; for 2h; | 4-chloro-2-nitrophenyl)methanol (40.0 g, 0.21 mol) was dissolved in ethanol (700 mL) and hydrogenated under hydrogen gas (20 psi) in the presence of 5% platinum on sulfided carbon (Pt-C/S, 5.00g). After 2 hours the catalyst was removed by filtration through Celite and the solvent removed under reduced pressure. This provided the desired compound (2-amino-4-chlorophenyl)methanol (32.9 g) which was used without further purification. HPLC Rt =1.70 minutes. 1H NMR (CDCl3) delta 6.96 (d, 1H), 6.67 (m, 2H), 4.64 (s, 2H), 4.27 (bs, 2H), 1.56 (bs, 1H). |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
With hydrogen; In methanol; | A. 5-Chloro-2-hydroxymethyl aniline To a solution of 4-chloro-2-nitro benzyl alcohol (25.00 g) in methanol (1 ltr) under nitrogen at room temperature, was added platinum on sulfided carbon (2.5 g, 10% by wt). The reaction mixture was shaken under 50 psi of hydrogen until the theoretical uptake of hydrogen had occurred. Filtration, then removal of the solvent in vacuo afforded the desired compound as a solid (21.00 g). delta (360 MHz, DMSO-d6) 4.35 (2H, d, J=4.95 Hz, CH2 OH), 5.17 (1H, t, J=4.95 Hz, CH2 OH), 6.77 (1H, dd, J=7.98 Hz, J=2.18 Hz, 4-H), 7.06 (1H, d, J=2.18 Hz, 6-H), 7.18 (1H, d, J=7.98 Hz, 3-H), 8.08 (1H, bs, NH2), 8.47 (1H, bs, NH). |