HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → Methyl 4-iodo-2-[(4-methoxy-4-oxobutanoyl)amino]benzoate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Butanoic acid, 4-chloro-4-oxo-, methyl ester | HCID 73888 | — |
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | Methyl 2-amino-4-iodobenzoate | HCID 18929930 | — |
| Catalyst | 4-(Dimethylamino)pyridine | HCID 14284 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | Methyl 4-iodo-2-[(4-methoxy-4-oxobutanoyl)amino]benzoate | HCID 58476671 | 102.6% |
Reaction Steps
To a solution of methyl 2-amino-4-iodobenzoate (17 g, 61.3 mmol) in DCM (200 mL), was added DIEA (10.6 mL, 64.4 mmol) and DMAP (37.5 mg, 0.31 mmol). To this solution was added 3-(carbomethoxy)propionyl chloride (8.3 mL, 67.4 mmol) dropwise, and the reaction mixture was allowed to stir at rt for 2 h. To the reaction mixture was then added H2O (80 mL) and the mixture was allowed to stir for 30 min. The organic solution was separated and the aqueous solution was extracted with DCM (2×100 mL). The organic solutions were combined, washed with H2O (2×100 mL) and brine (1×100 mL), dried over Na2SO4, filtered and concentrated to give methyl 4-iodo-2-[(4-methoxy-4-oxobutanoyl)amino]benzoate (24.6 g, 99%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08268992B2 |
| Source dataset | uspto-grants-2012_09 |
| ORD ID | ord-e96ee3e4af2940ea82cd7e432d54a515 |
| Source note | uspto-grants-2012_09 |