HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Carbonate → HCID 89647654, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Carbonate | HCID 10340 | — |
| Reactant | Ethyl chloroformate | HCID 10928 | — |
| Reactant | 3-Chloro-D-phenylalanine | HCID 7009409 | — |
| Solvent | Methanol--water (1/1) | HCID 22242641 | — |
| Product | HCID 89647654 | HCID 89647654 | — |
Reaction Steps
Na2CO3 (2.12 g, 20.04 mmol) was added to a suspension of 3-chloro-D-phenylalanine 9 (2.6 g, 10.02 mmol) in MeOH/H2O (8.3 mL/8.3 mL) at room temperature. Ethyl chloroformate (1.44 mL, 15.03 mmol) was added drop wise over 20 min via syringe pump and the reaction was stirred overnight. The reaction mixture was washed with Et2O (1×15 mL) and the aqueous layer was acidified to pH ˜5 with 2 M HCl (aq). The aqueous layer was extracted with EtOAc (2×30 mL). The combined organics were washed with brine, dried over MgSO4, filtered and concentrated to obtain the ethyl carbamate.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09062071B2 |
| Source dataset | uspto-grants-2015_06 |
| ORD ID | ord-9af57227ae194a44a834b854a7c61f9d |
| Source note | uspto-grants-2015_06 |