Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Pyridine | HCID 1049 | — |
| Reactant | Lithium borohydride | HCID 4148881 | — |
| Reactant | HCID 86588730 | HCID 86588730 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 86588729 | HCID 86588729 | 66% |
Reaction Steps
3.69 g (0.009 mol) of tert-butyl [4′-(2,4-dioxothiazolidin-5-ylidenemethyl)biphenyl-3-yl]methylcarbamate, 6 ml of THF and 7.3 ml of pyridine are introduced, in order, into a 50 ml three-necked round-bottomed flask. The mixture is placed under nitrogen and 10 ml of a freshly prepared 2 M LiBH4 solution (0.02 mol) in THF are added dropwise. After stirring for 30 minutes at room temperature, the mixture is heated under reflux for 16 hours. The reaction medium is poured over 32 ml of a 1 N HCl solution and the THF is evaporated under vacuum. The precipitate obtained is filtered. After drying, the crude product (2.75 g) is chromatographed on 95 g of silica gel, eluting with a heptane/ethyl acetate=3/7 mixture. 2.45 g (66%) of tert-butyl [4′-(2,4-dioxothiazolidin-5-ylmethyl)biphenyl-3-yl]methylcarbamate are obtained.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US07294639B2 |
|---|
| Source dataset | uspto-grants-2007_11 |
|---|
| ORD ID | ord-8df4db5e6e2f4b2780a40d3ef921c6e1 |
|---|
| Source note | uspto-grants-2007_11 |
|---|