HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → 3-[1-(4-Chlorobenzyl)-3-(t-butylthio)-5-methoxyindol-2-yl]-2,2-dimethylpropanoic acid methyl ester
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Sodium Acetate | HCID 517045 | — |
| Reactant | Methyl 5-t-butylthio-2,2-dimethyl-4-oxopentanoate | HCID 14980531 | — |
| Reactant | 1-(4-Chlorobenzyl)-1-(4-methoxyphenyl)hydrazine hydrochloride | HCID 18947569 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | 3-[1-(4-Chlorobenzyl)-3-(t-butylthio)-5-methoxyindol-2-yl]-2,2-dimethylpropanoic acid methyl ester | HCID 11762500 | — |
Reaction Steps
To a solution of 39 g of methyl 5-(t-butylthio)-2,2-dimethyl-4-oxopentanoate in a mixture of 300 mL of toluene and 150 mL of glacial acetic acid was added 15 g of NaOAc and 50 g of 1-(4-methoxyphenyl)-1-(p-chlorobenzyl)hydrazine hydrochloride. The reaction was maintained with stirring at room temperature for 3 days under argon in the dark. The mixture was poured into 3 L of H2O and extracted with 3×500 mL of EtOAc. The ethyl acetate was washed with 3×500 mL of water then solid NaHCO3 was added. The mixture was filtered and the filtrate washed twice with water. The organic phase was dried over MgSO4 and evaporated to dryness to provide the title compound. m.p. 102°-103° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05321033 |
| Source dataset | uspto-grants-1994_06 |
| ORD ID | ord-a5b48dfdc77e43eab7ebf3c83c7e4abf |
| Source note | uspto-grants-1994_06 |