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CAS No. : | 22080-96-2 | MDL No. : | MFCD01407645 |
Formula : | C9H10O4 | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | HZWPJAZIRZFCGX-UHFFFAOYSA-N |
M.W : | 182.17 | Pubchem ID : | 529894 |
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 |
---|---|---|
56% | With di-isopropyl azodicarboxylate; triphenylphosphine; In tetrahydrofuran; at 20℃; for 20h;Cooling with ice; | To the ice-cooled solution of 2 , 6-dimethoxy-4- [ (2-methyl-3- phenylphenyl) methoxy] benzaldehyde 14 (0.92 g, 5.04 mmol) , triphenylphosphine (1.45 g, 5.55 mmol) and compound 4 (1.0 g, 5.04 mmol) in dry THF (21 mL) , diisopropyl azodicarboxylate (DIAD) (1.08 mL, 5.55 mmol) in THF (21 mL) was added dropwise. The resulting yellow solution was allowed to warm to room temperature and stirred for additional 20 h. The mixture was concentrated under reduced pressure. The residue was purified by flash chromatography on silica gel using 0-60% ethyl acetate in hexane as colourless solid (1.02 g, yield: 56%). mp: 161.5-162.0 C; 1H NMR (600 MHz, DMSO-d6) delta[ ppm] : 10.37 (s, 1H) , 7.44-7.40 (m, 3H) , 7.37 (m, 1H) , 7.32 -7.28 (m, 4H) , 6.20 (s, 2H) , 5.16 (s, 2H) , 3.89 (s, 6H) , 2.27 (s, 3H) ; 13C NMR (151 MHz, DMSO-d6) delta [ppm]: 187.9, 165.6, 164.3, 143.4, 141.9, 134.7, 134.3, 130.8, 129.5, 128.5, 128.3, 127.1, 125.9, 109.1, 91.1, 69.7, 56.2, 16.4; IR V (ATR cm-1) 3013, 2936, 1668, 1607, 1607, 1582, 1465, 1166; HRMS (ESI-TOF) Calcd C23H2204 [M+Na]+ : 385.1416; found [M+Na]+ : 385.1420 |
With di-isopropyl azodicarboxylate; triphenylphosphine; In tetrahydrofuran; at 0 - 20℃; | Diisopropyl azodicarboxylate (2.158 mL, 11.10 mmol) in THF (50 mL) was added dropwise to a cooled (0 C) solution of 4-hydroxy-2,6-dimethoxybenzaldehyde (1.838 g, 10.09 mmol), triphenylphosphine (2.91 g, 11.10 mmol) and 2-methyl-[l,l'- biphenyl]-3-yl)methanol (2 g, 10.09 mmol) in dry THF (50 mL). The resulting yellow solution was allowed to slowly warm to room temperature with stirring overnight. 1H NMR (500MHz, CHLOROFORM-d) delta 10.40 (s, 1H), 7.48-7.42 (m, 3H), 7.40 (d, J=7.6 Hz, 1H), 7.36-7.30 (m, 4H), 6.23 (s, 2H), 5.19 (s, 2H), 3.94-3.89 (m, 6H), 2.30 (s, 3H). Rf = 0.55 1 : 1 ethyl acetate :hexanes. |
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