Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | Oxalyl chloride | HCID 65578 | — |
| Reactant | HCID 58399171 | HCID 58399171 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 58399162 | HCID 58399162 | — |
Reaction Steps
To a solution of 0.9 g of the product of Step 9 in 50 mL of CH2Cl2 was added 0.42 mL of oxalyl chloride at 0° C. After stirring for 1 h at 0° C., 4 mL of MeOH was added and the mixture was stirred for another hour and quenched with 30 mL of saturated aqueous solution of NaHCO3. The mixture was extract with 50 mL of CH2Cl2 and the extract was dried over Na2SO4. After filtration, the filtrated was concentrated to give 1.2 of the title product as a solid. 1H NMR (500 MHz, acetone-d6) d 8.11 (m, 2H), 7.92 (m, 1H), 7.45-7.52 (m, 3H), 7.28-7.34 (m, 2H, 4.70 (m, 1H), 7.32 (m, 1H), 4.12 (t, 1H), 3.97 (s, 3H), 3.48-3.55 (m, 1H), 3.08-3.07 (m, 1H), 3.00 (s, 3H), 2.10 (m, 1H), 1.76 (m, 1H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07696222B2 |
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| Source dataset | uspto-grants-2010_04 |
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| ORD ID | ord-d3e21e2f9bc74f0b9a8a8150c0cfdb6c |
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| Source note | uspto-grants-2010_04 |
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