HuagongsheHuagongshe Chemistry Print Report · For research reference only
1,2-Dichloroethane → HCID 23138332, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1,2-Dichloroethane | HCID 11 | — |
| Reactant | Acetic Acid | HCID 176 | — |
| Reactant | 1-Benzylpiperazine | HCID 75994 | — |
| Reactant | tert-butyl N-(2-oxoethyl)carbamate | HCID 4247255 | — |
| Reactant | Sodium triacetoxyborohydride | HCID 5049666 | — |
| Product | HCID 23138332 | HCID 23138332 | 61% |
Reaction Steps
To a solution of 1-benzylpiperazine (4.4 g), tert-butyl N-(2-oxoethyl)carbamate (3.8 g) and acetic acid (1.7 ml) in 1,2-dichloroethane (50 ml) was added sodium triacetoxyborohydride (8.1 g) under ice-cooling. The reaction mixture was mixed at room temperature for 2 days. Then, the reaction solution washed with an aqueous potassium carbonate solution and dried over anhydrous magnesium sulfate. The solvent was distilled off under reduced pressure, and the residue was dissolved in methanol (50 ml). A 4 N solution of hydrogen chloride in ethanol (40 ml) was added thereto, and mixed at room temperature for 5 hours. The precipitate was collected by filtration and washed with diethyl ether and hexane to obtain the title compound (5.0 g, 61%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07820673B2 |
| Source dataset | uspto-grants-2010_10 |
| ORD ID | ord-c18924fa5cb045acac8b0e78eee5e729 |
| Source note | uspto-grants-2010_10 |