Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Dimethylformamide | HCID 6228 | — |
| Reactant | HCID 23119569 | HCID 23119569 | — |
| Reactant | HCID 178418306 | HCID 178418306 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Solvent | Ether tetrahydrofuran | HCID 21868444 | — |
| Product | HCID 87516624 | HCID 87516624 | 73.3% |
Reaction Steps
To a stirred solution of 4bromo-1-p-methoxyphenylsulfonyl-2-(3,4,5-trimethoxyphenyl)-pyrrole (0.30 g, 0.62 mmol, Example 94b) in ethyl ether/THF (5 ml, 1:1 v/v) tert-butyl-lithium (1.5 equiv., 1.7 M in pentane) is added at −78° C. The reaction mixture is stirred for 20 min at −78° C., and DMF (255 mg, 5 equiv.) is added drop wise. The reaction mixture is kept for 1 h at −78° C., allowed to come to 4° C., and poured onto ice, 1 M aqueous HCl and ethyl acetate. The organic layer is dried (MgSO4), the solvents are evaporated, and the residue chromatographed on SiO2 with ethyl acetate/hexane to yield the title compound (0.196 g, 73%) as a light yellow solid. 1H-NMR (300 MHz, DMSO-d6): 9.86 (s, CHO); 8.44 (d, J=1.9, 1H); 7.38 (d, J=9.0, 2H); 7.01 (d, J=9.0, 2H); 6.56 (d, J=1.9, 1H); 6.36 (s, 2H); 3.82 (s, MeO); 3.72 (s, MeO); 3.67 (s, 2MeO).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07612064B2 |
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| Source dataset | uspto-grants-2009_11 |
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| ORD ID | ord-23fe3cdfc32248d49f2a3c5715d6b510 |
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| Source note | uspto-grants-2009_11 |
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