HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Bicarbonate → Tert-Butyl 4-(4-Amino-2-Chlorophenyl)Piperazine-1-Carboxylate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | Tert-butyl 4-(2-chloro-4-nitrophenyl)piperazine-1-carboxylate | HCID 18783805 | — |
| Reactant | MeOH tetrahydrofuran | HCID 21899815 | — |
| Catalyst | Zinc | HCID 23994 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Product | Tert-Butyl 4-(4-Amino-2-Chlorophenyl)Piperazine-1-Carboxylate | HCID 18783766 | — |
Reaction Steps
To a solution of the product of Example 18A (1.5 g, 4.4 mmol) in 1:1 tetrahydrofuran/methanol (80 mL) at ambient temperature was slowly added zinc power (1.43 g, 22 mmol) and acetic acid (5 mL). The mixture was stirred for 1 hour, and saturated aqueous sodium hydrogen carbonate solution was added. The mixture was stirred for 1 hour and filtered, and extracted with ethyl acetate. The organic layer was washed with brine, dried over anhydrous sodium sulfate, filtered, and concentrated. The residue was purified by flash chromatography on silica gel eluting with 5/1 petroleum ether/ethyl acetate to give title compound. MS: 312 (M+H+).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09212192B2 |
| Source dataset | uspto-grants-2015_12 |
| ORD ID | ord-87eb4341f5dd46bf9f8137cf8654aa52 |
| Source note | uspto-grants-2015_12 |