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CAS No. : | 108298-35-7 | MDL No. : | |
Formula : | C12H14O5 | Boiling Point : | - |
Linear Structure Formula : | - | InChI Key : | - |
M.W : | 238.24 | Pubchem ID : | - |
Synonyms : |
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Signal Word: | Class: | ||
Precautionary Statements: | UN#: | ||
Hazard Statements: | Packing Group: |
* 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 |
---|---|---|
90% | at 200℃; for 2h; | |
89% | at 180 - 200℃; | |
76% | at 180 - 210℃; for 1.5h; | 5 A mixture of compound K (41.4 g, 295 mmol) and dimethyl but-2-ynedioate (47.2 mL, 384 mmol) was stirred at 180 0C for 1 hour, then at 210 0C for 30 minutes. The mixture was cooled to room temperature and purified by silica gel chromatography (ethyl aceate : hexane = 20 : 1 - 4 : 1 ) to give compound L (53.4 g, 76%) as a pale-yellow oil. 1H NMR (CDCl3, 400MHz) : δ 2.34 (3H, s), 3.84 (3H, s), 3.88 (3H, s), 3.90 (3H, s), 6.91 (IH, d, J - 2.4 Hz), 7.29 (IH, d, J = 2.4 Hz). EIMS (+) : 238 [M]+ |
73% | In neat (no solvent) at 180 - 210℃; for 3h; | |
66% | 1.) 180 deg C, 1 h, 2.) 210 deg C, 2 h; | |
35% | With benzophenone In acetone at -20 - -10℃; for 5h; Irradiation; |
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
70% | at 180 - 210℃; for 3h; Neat (no solvent); | 5 4-methoxy-6-methyl-pyran-2-one Compound 5a (25.3 g, 180.5 mmol) in DMAD (neat, 33.3 mL, 271.0 mmol) was heated in a round bottom flask at 180 0C for 1 hr and then at 210 °C for 2 hrs. The reaction mixture was cooled to room temperature and concentrated onto SiO2 (75 g), then purified via column chromatography (Horizon, 65% to 60% gradient starting with 5% EtOAc/Hexanes to 20% EtOAc/Hexanes) to afford 5-methoxy-3-methyl-phthalic acid dimethyl ester Compound 5b (30.12 g, 70%) as a colorless oil. 1H NMR (300 MHz, CDCl3) δ 7.29, (d, J = 2.1 Hz, IH), 6.91 (d, 2.0Hz, IH), 3.99 (s, 3H), 3.90 (s, 3H), 3.84 (s, 3H), 234 (s, 3H). |