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CAS No. : | 1016-58-6 | MDL No. : | MFCD00014701 |
Formula : | C9H11NO5 | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | WBSCOJBVYHQOFB-UHFFFAOYSA-N |
M.W : | 213.19 | Pubchem ID : | 66097 |
Synonyms : |
|
Signal Word: | Warning | Class: | N/A |
Precautionary Statements: | P280-P305+P351+P338 | UN#: | N/A |
Hazard Statements: | H302 | 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 |
---|---|---|
98% | With thionyl chloride; triethylamine; In dichloromethane; at 0 - 20℃; for 12h; | Step (b): To a solution of (4,5-dimethoxy-2-nitrophenyl)methanol (19.5 g, 91 mmol) in CH2Cl2 (55 mL) was added a few drops of triethylamine, and SOCl2 (1.3 mL, 18 mmol) at 0 C. After stirring overnight at room temperature, the reaction was quenched by addition of EtOH. The organic layer was washed with water and brine, dried over Na2SO4, filtered off and concentrated under reduced pressure. After purification by column chromatography on silica gel (Cyclohexane/EtOAc 7:3), the pure product 1 (20.7 g, 90 mmol) was obtained as a yellow solid. Yield, 98%. m.p: 59.9 C. 1H NMR (250 MHz, CDCl3) δ 7.68 (s, 1H), 7.09 (s, 1H), 5.00 (s, 2H), 4.00 (s, 3H), 3.96 (s, 3H). 13C NMR (100 MHz, CDCl3) δ 153.5, 148.8, 140.4, 127.3, 112.9, 108.5, 56.6, 56.5, 43.7. |
86.4% | With thionyl chloride; In (2S)-N-methyl-1-phenylpropan-2-amine hydrate; | Preparation of 2-nitro-4,5-dimethoxybenzyl chloride 570 g of 2-nitro-4,5-dimethoxybenzyl alcohol was added over 1 hour to 733 ml of thionyl chloride at 0 C. The solution was heated to 25 C. over 2 hours and to 50-56 C. for 2 hours. The solution was cooled to 5 C. and the mixture was poured onto 12 l of ice water with stirring. The supernatant was poured off and the solid washed with water. The oily solid was blended with ice and water, filtered, and dried in a 40 C. vacuum oven to yield 535 g, 86.4% yield. |
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