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CAS No. : | 2423-71-4 | MDL No. : | MFCD00007339 |
Formula : | C8H9NO3 | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | FNORUNUDZNWQFF-UHFFFAOYSA-N |
M.W : | 167.16 | Pubchem ID : | 17030 |
Synonyms : |
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Signal Word: | Warning | Class: | N/A |
Precautionary Statements: | P261-P305+P351+P338 | UN#: | N/A |
Hazard Statements: | H315-H319-H335 | Packing Group: | N/A |
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 |
---|---|---|
86% | With hydrogen;palladium 10% on activated carbon; In ethanol; under 1125.11 Torr; for 1h; | A solution of 1 g (6 mmol) of 2,6-dimethyl-4-nitrophenol in 20 ml of ethanol is placed under 1.5 bar of hydrogen in the presence of 10% Pd/C for 1 hour. The Pd/C is eliminated by filtration on celite and the filtrate is concentrated under reduced pressure. The evaporation residue crystallizes spontaneously, it is washed twice with 50 ml of heptane and dried overnight under vacuum. A cream coloured solid is obtained with a yield of 86%. [00525] Melting point: 139-140 C. |
85% | With hydrogen;palladium 10% on activated carbon; In methanol; at 20℃; under 2250.23 Torr; | Step 1: 4-amino-2,6-dimethyl-phenol; 3.00 g (18.0 mmol) 2,6-dimethyl-4-nitrophenol were hydrogenated with 0.50 g palladium on charcoal (Pd/C, 10%) in 50 mL MeOH in a 3 bar hydrogen atmosphere at RT. After the end of the reaction the catalyst was suction filtered and the filtrate was concentrated by rotary evaporation. The residue was triturated with DIPE and the precipitate was suction filtered and dried i. vac.Yield: 2.10 g (85% of theory)ESI-MS: m/z=138 (M+H)+ Rf: 0.5 (silica gel: DCM/MeOH/cyc/NH4OH=70:15:15:2) |
79% | With hydrogenchloride; tin; acetic acid; at 20℃; for 48h; | 4-Amino-2,6-dimethylphenol (15). Thesynthesis was carried out according to the methodology described in theliterature.5 2,6-Dimethyl-4-nitrophenol (0.60 g, 3.0 mmol), solidtin (1.14 g, 9.6 mmol), hydrochloric acid (0.72 mL), and acetic acid (7.2 mL)were placed in a round-bottomed flask. The system was kept under magneticstirring for 48 h at room temperature. Distilled water (60 mL) and aqueousNaHCO3 were added for neutralization and the product was extractedfrom the aqueous phase with ethyl acetate (100 mL). The organic phase waswashed with aqueous saturated NaHCO3, dried with MgSO4,filtered, and rotary-evaporated. The product was a red solid (0.33 g; 79% yield) withm.p. 107-109 C. IR (KBr, ν max/cm-1):3420, 3388 (N-H), 2949, 2919, 2853 (C-H), 1632, 1487 (C=C), 1234, 1205 (C-O,C-N). 1H NMR (200 MHz, CDCl3) δ/ppm: 7.13 (1H, s, OH), 6.15 (2H, s, Ar-H), 4.30 (2H, s,NH2), 2.01 (6H, s, 2×CH3). |
With hydrogen;palladium 10% on activated carbon; In ethanol; at 20℃; for 4h; | A suspension of 50 g of 4-nitro-2,6-dimethylphenol (MW=167.16; 294.5 mmol) and 5 g of 10% palladium-on-charcoal (MW=106.41; 4.7 mmol) in 1000 ml of ethanol was stirred at room temperature under a hydrogen atmosphere in a Parr hydrogenator for 4 hours. The mixture was then filtered under nitrogen through a layer of Celite and the solvent was evaporated off under reduced pressure.The solid residue thus obtained was 4-amino-2,6-dimethylphenol (38 g), which was used in subsequent reactions without further purification.LC/MS (M+H)+=138; 123 (base peak).1H-NMR (δ, DMSO d-6) 7.5-6.8 (broad s, 1H); 6.16 (s, 2H); 4.5-3.9 (broad s, 2H); 2.03 (s, 6H). | |
With hydrogen;palladium 10% on activated carbon; In ethanol; at 20℃; for 4h; | A suspension of 50 g of 4-nitro-2,6-dimethylphenol (MW = 167.16; 294.5 mmol) and 5 g of 10% palladium-on-charcoal (MW = 106.41 ; 4.7 mmol) in 1000 ml of ethanol was stirred at room temperature under a hydrogen atmosphere in a Parr hydrogenator for 4 hours. The mixture was then filtered under nitrogen through a layer of Celite and the solvent was evaporated off under reduced pressure.The solid residue thus obtained was 4-amino-2,6-dimethylphenol (38 g), which was used in subsequent reactions without further purification.LC/MS (M+H)+ = 138; 123 (base peak).1H-NMR (δ, DMSO d-6) 7.5-6.8 (broad s, 1 H); 6.16 (s, 2H); 4.5-3.9 (broad s, 2H); 2.03 (s, 6H). |
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