HuagongsheHuagongshe Chemistry Print Report · For research reference only
Diisopropylethylamine → 1-Tert-butoxycarbonyl-3-benzhydrylpiperazine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | Carbonic acid, bis(1,1-dimethylethyl) ester | HCID 10219638 | — |
| Reactant | 2-Benzhydrylpiperazine dihydrochloride | HCID 22674743 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | 1-Tert-butoxycarbonyl-3-benzhydrylpiperazine | HCID 22674800 | 70.5% |
Reaction Steps
Di-tert-butyl carbonate (996 mg) was added to a mixture of 2-benzhydrylpiperazine dihydrochloride (1.65 g) and N,N-diisopropylethylamine (3.5 ml) in N,N-dimethylformamide (17 ml) under ice-cooling. After being stirred at same temperature for 2 hours, the mixture was poured into ice-water and extracted with ethyl acetate. The extract was washed with brine, dried over sodium sulfate and evaporated under reduced pressure to give a crude oil. The oil was purified by column chromatography on silica gel using a mixed solvent of dichloromethane and methanol (50:1) to give 1-tert-butoxycarbonyl-3-benzhydrylpiperazine (1.26 g) as a colorless powder.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06787543B2 |
| Source dataset | uspto-grants-2004_09 |
| ORD ID | ord-a028d704e8994664bedbc37322bf8650 |
| Source note | uspto-grants-2004_09 |