HuagongsheHuagongshe Chemistry Print Report · For research reference only
Citric Acid → HCID 66925750, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Citric Acid | HCID 311 | — |
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | Benzotriazol-1-yloxy-tris(dimethylamino)phosphonium hexafluorophosphate | HCID 151348 | — |
| Reactant | Tert-butyl 1,4-diazepane-1-carboxylate | HCID 2756058 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 66925750 | HCID 66925750 | — |
Reaction Steps
A mixture of the product of example 10a (340 mg), tert-butyl 1,4-diazepane-1-carboxylate (694 μl), DIPEA (2.4 ml) and BOP (1.9 g) in dichloromethane (15 ml) was stirred for 18 h at room temperature. The reaction mixture was poured into an aqueous citric acid solution (5%) and extracted with ethyl acetate. The organic layer was dried (MgSO4), filtered and concentrated in vacuo. The residue was purified by chromatography on silica gel in toluene/acetone [1/0→7/3 (v/v)] as eluent.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08394789B2 |
| Source dataset | uspto-grants-2013_03 |
| ORD ID | ord-0a3bdfd907da4a2a80c17ef8ae1a9cb2 |
| Source note | uspto-grants-2013_03 |