HuagongsheHuagongshe Chemistry Print Report · For research reference only
Benzyl chloroformate → Benzyl 3-bromopropylcarbamate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Benzyl chloroformate | HCID 10387 | — |
| Reactant | 3-Bromopropylamine hydrobromide | HCID 78701 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Solvent | Sodium Hydroxide | HCID 14798 | — |
| Product | Benzyl 3-bromopropylcarbamate | HCID 254436 | 105.3% |
Reaction Steps
Benzylchloroformate (8.6 ml, 60 mmol) was added to a stirred mixture of 3-bromopropylamine hydrobromide (6.6 g, 30 mmol) in methylene chloride (100 ml) and 3N sodium hydroxide solution (100 ml) at 0° C. After stirring two phase reaction mixture at room temperature for overnight, organic layer was separated and washed with water twice (30 ml×2). After drying with MgSO4, the volatile solvent was evaporated under reduced pressure. The residue was purified with silica gel column chromatography (EtOAc:Hx=1:4) to obtain desire compound (8.6 g, 98%) as colorless oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08895558B2 |
| Source dataset | uspto-grants-2014_11 |
| ORD ID | ord-8d5f0cc8a2fd49aa9f4c3dc927ecccc8 |
| Source note | uspto-grants-2014_11 |