HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → Methyl 4-[3-amino-5-chloro-3-(2-chlorophenyl)-2,3-dihydro-2-oxoindol-1-yl]methyl-3-methoxybenzoate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | Methyl 4-(bromomethyl)-3-methoxybenzoate | HCID 2759828 | — |
| Reactant | 3-Amino-5-chloro-3-(2-chlorophenyl)-1,3-dihydroindol-2-one | HCID 19076376 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | Methyl 4-[3-amino-5-chloro-3-(2-chlorophenyl)-2,3-dihydro-2-oxoindol-1-yl]methyl-3-methoxybenzoate | HCID 19076628 | — |
Reaction Steps
A solution of 1.13 g of 3-amino-5-chloro-3-(2-chlorophenyl)-1,3-dihydroindol-2-one in 7 ml of DMF is cooled to 0° C. under an argon atmosphere and 0.120 g of sodium hydride as an 80% dispersion in oil is added. After stirring for 30 minutes, 1 g of methyl 4-bromomethyl-3-methoxybenzoate is added and the reaction mixture is stirred for 1 hour at 0° C. It is poured into water and the precipitate formed is filtered off, washed with water, taken up with AcOEt, dried over sodium sulfate and evaporated under vacuum. The residue is chromatographed on silica using a DCM/AcOEt mixture (93/7; v/v) as the eluent to give the expected product after crystallization from a DCM/iso ether mixture. m=1.88 g. M.p.=152° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05594023 |
| Source dataset | uspto-grants-1997_01 |
| ORD ID | ord-26f778bfe2804b99ad694e087972b992 |
| Source note | uspto-grants-1997_01 |