HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethyl chloroacetate → HCID 18623221, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethyl chloroacetate | HCID 7751 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | 2-Amino-2-(3,4-difluorophenyl)ethanol | HCID 22048878 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 18623221 | HCID 18623221 | — |
Reaction Conditions
| Temperature | 0 °C |
|---|
Reaction Steps
To a suspension of NaH (8.0 mmol, 0.19 g) in 10 mL THF at 0° C. was added a solution of 2-amino-2-(3,4-difluorophenyl)-ethanol (7.51 mmol, 1.3 g) in 20 THF dropwise via an addition funnel and after 30 min ethyl chloroacetate was added dropwise via syringe. The orange colored reaction mixture was stirred for 2 hours at 0° C. and then for 2 hours at 35° C. The solvent was removed and the 5-(3,4-difluoro-phenyl)-morpholin-3-one was isolated as a thick yellow oil (0.5 g). 1H NMR showed that the product was about 85% pure and any attempts to purify it further by column chromatography were not successful. It was used in the next reaction as described below without further purification.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06362182B1 |
| Source dataset | uspto-grants-2002_03 |
| ORD ID | ord-d8bb694e3a254c848a822cab6ff9f87c |
| Source note | uspto-grants-2002_03 |