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CAS No. : | 80866-75-7 | MDL No. : | MFCD00007171 |
Formula : | C8H9NO3 | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | KOVQGYQQVNCUBR-UHFFFAOYSA-N |
M.W : | 167.16 | Pubchem ID : | 591360 |
Synonyms : |
|
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 |
---|---|---|
89.9% | With borane-THF; In tetrahydrofuran; at 0 - 20℃; for 3h;Inert atmosphere; | To a solution of 3-methyl-4-nitro-benzoic acid (2 g, 11.04 mmol, 1 eq) in anhydrous THF (20 mL) was added BH3-THF (1 M, 27.60 mL, 2.5 eq) at 0-5 C. under N2 atmosphere. The mixture was stirred at 20 C. for 3 h. The reaction mixture was quenched by addition of MeOH (30 mL) at 20 C. then stirred at 20 C. for 0.5 h. The mixture was concentrated to afford the crude product (3-methyl-4-nitro-phenyl)methanol (1.66 g, 9.93 mmol, 89.9% yield, 100% purity) as an off-white solid which was used in the next step without further purification. 1H NMR (400 MHz, CD3OD) δ ppm 7.97 (d, J=8.3 Hz, 1H), 7.46-7.35 (m, 2H), 4.90 (s, 2H), 2.59 (s, 3H); ES-LCMS m/z 168.2 [M+H]+. |
67 g | With Trimethyl borate; dimethylsulfide borane complex; In tetrahydrofuran; methanol; dichloromethane; at 65℃; for 6h;Inert atmosphere; | A flask purged with nitrogen was charged with 3-methyl-4-nitro-benzoic acid (72.5 g, 0.400 mol), trimethyl borate (166.2 g, 1.600 mol) and dry tetrahydrofuran (1449 mL). A solution of borane dimethyl sulfide complex (63.8 g, 79.8 mL, 0.840 mol) was added drop-wise to the stirred batch at 20-35 C. over at least 30 min. An exotherm and effervescence were observed during the addition. The mixture was stirred at 65 C. for at least 6 h or until in-process HPLC analysis showed that conversion was greater than 97%. Reaction was quenched at 20-40 C. with cooling by drop-wise addition of methanol (46 mL) followed by aq 5 N hydrochloric acid (144 mL) over at least 30 min. Exotherm and effervescence were observed during the quench. After stirring the batch at 50 C. for at least 1 h, it was concentrated under reduced pressure to a volume of 360 mL. The concentrated batch was washed with water (453 mL) and the solids were collected on a filter. The wet filter cake was dissolved in CH2Cl2 (2170 mL) at and the resulting solution dried over anhydrous magnesium sulfate (36 g). The dried filtrate solution containing the title compound (67 g, 100% yield) was used directly in the preparation of 3-methyl-4-nitro-benzaldehyde. |
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