HuagongsheHuagongshe Chemistry Print Report · For research reference only
HRID 1021534Generated: October 31, 2026
Oxalyl chloride → Ethyl 6-chloro-7-(4-(1-(4-chlorophenyl)-3-hydroxypropan-2-ylcarbamoyl)phenoxy)chroman-4-carboxylate
https://huagongshe.com/reaction/1021534
Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Oxalyl chloride | HCID 65578 | — |
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | beta-Amino-4-chlorobenzenepropanol | HCID 548289 | — |
| Reactant | 4-(6-Chloro-4-(ethoxycarbonyl)chroman-7-yloxy)benzoic acid | HCID 58244395 | — |
| Catalyst | Dimethylformamide | HCID 6228 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | Ethyl 6-chloro-7-(4-(1-(4-chlorophenyl)-3-hydroxypropan-2-ylcarbamoyl)phenoxy)chroman-4-carboxylate | HCID 67167139 | 76.82% |
Reaction Steps
To a solution of 4-(6-chloro-4-(ethoxycarbonyl)chroman-7-yloxy)benzoic acid (0.100 g, 0.2654 mmol) in dichloromethane (1.5 ml) and DMF (1 drop) was added oxalyl dichloride (0.02778 ml, 0.3185 mmol), and the reaction was stirred for 30 minutes. N-ethyl-N-isopropylpropan-2-amine (0.1112 ml, 0.6370 mmol) and 2-amino-3-(4-chlorophenyl)propan-1-ol (0.06405 g, 0.3450 mmol) were added, and the reaction was stirred for 16 hours. The reaction was diluted with EtOAc and washed with 1M hydrochloric acid, saturated sodium bicarbonate, and saturated sodium chloride. The organic layer was dried over anhydrous sodium sulfate, filtered, and concentrated. The crude material was purified on a Biotage SP1 system eluting with 25-100% EtOAc in hexanes to yield 111 mg of the title compound (76.82% yield).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US08716498B2 |
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| Source dataset | uspto-grants-2014_05 |
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| ORD ID | ord-3250da268497440e90519283666f87d1 |
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| Source note | uspto-grants-2014_05 |
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