HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Dithionite → HCID 12069414, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Dithionite | HCID 24489 | — |
| Reactant | 1,4-Dioxane | HCID 31275 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | tert-butyl N-(5-chloro-2-nitrophenyl)-N-methylcarbamate | HCID 15544598 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 12069414 | HCID 12069414 | 55.5% |
Reaction Steps
A mixture of N-(2-nitro-5-chlorophenyl)-N-methylcarbamic acid t-butyl ester (6.0 g), dioxane (150 ml), water (30 ml), sodium hydrosulfite (14.6 g) and sodium hydrogencarbonate (17.6 g) was heated under reflux for 30 minutes. The reaction mixture was partitioned between ethyl acetate and water. The extract was washed with saturated aqueous sodium chloride solution, dried over anhydrous sodium sulfate and then concentrated. The residue was chromatographed on a silica gel column using ethyl acetate/n-hexane (1/3) as the eluant to afford the title compound (2.98 g). Rf=0.23 (thin-layer chromatography on a silica gel plate using ethyl acetate/n-hexane (1/3) as the eluant).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06569877B2 |
| Source dataset | uspto-grants-2003_05 |
| ORD ID | ord-39d4eda23219442bac3081b0e0a9de19 |
| Source note | uspto-grants-2003_05 |