HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethanolamine → benzyl N-(2-hydroxyethyl)carbamate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethanolamine | HCID 700 | — |
| Reactant | Benzyl chloroformate | HCID 10387 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | benzyl N-(2-hydroxyethyl)carbamate | HCID 280458 | 70% |
Reaction Steps
To a stirred solution of ethanolamine (4.0 g, 66 mmol) in DCM (4 mL) was added benzyl chloroformate (4.6 mL, 33 mmol) at 0° C. After 1 h, the reaction mixture was warmed to room temperature and washed with 1.0N HCl (40 mL) and water (40 mL). The organics were separated, dried with anhydrous sodium sulfate, filtered, and concentrated. To a solution of the crude product in ethyl acetate (30 mL) was added hexanes (30 mL). The resulting crystals were filtered and dried to give the title intermediate as a white solid (4.5 g, 70%). 1H NMR (CDCl3, 300 MHz) δ (ppm): 7.4-7.29 (m, 5H), 5.00 (s, 2H), 4.64 (t, J=5.5 Hz, 1H), 3.38 (q, J=6.0 Hz, 2H), 3.07 (t, J=6.0 Hz, 2H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07622508B2 |
| Source dataset | uspto-grants-2009_11 |
| ORD ID | ord-78202b3a1ed84814ac99f2e850264b23 |
| Source note | uspto-grants-2009_11 |