HuagongsheHuagongshe Chemistry Print Report · For research reference only
Diethylamine → HCID 10503756, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Diethylamine | HCID 8021 | — |
| Reactant | Isobutyl chloroformate | HCID 62365 | — |
| Reactant | HCID 10834544 | HCID 10834544 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 10503756 | HCID 10503756 | — |
Reaction Steps
To a solution of compound 51 (1.0 g, 2.5 mmol) in dry dichloromethane (10 mL) at −20° C. was added iso-butylchloroformate (450 mg, 3.3 mmol). After 20 min at −20° C. diethylamine (4 mL) was added and the reaction was allowed to warm to room temperature. After 1.5 hrs the solvent was evaporated and the reaction mixture was partitioned between ethyl acetate and water. The ethyl acetate was washed with water and brine and dried over MgSO4 and removed by evaporation. The crude product was purified by silica gel chromatography (0-60% ethyl acetate in heptanes) to give the product (compound 52) as white needles (800 mg, 73%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06187792B1 |
| Source dataset | uspto-grants-2001_02 |
| ORD ID | ord-7c85e7f412bc4501a3bbced03992c15c |
| Source note | uspto-grants-2001_02 |