HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → HCID 54327434, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | 2-Propylvaleryl chloride | HCID 76240 | — |
| Reactant | Alanine, methyl ester, hydrochloride (1:1) | HCID 2756298 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 54327434 | HCID 54327434 | 67.4% |
Reaction Steps
A solution of DL-alanine methyl ester hydrochloride (13.7 g, 98 mmole) and Et3N (20.2 g, 200 mmole) in water (50 ml) was added dropwise to an ice-cooled solution of valproyl chloride (15.0 g, 92 mmole) in CH2Cl2 (150 ml). After completion of addition the reaction mixture was stirred for 4 hrs. at RT. The layers were then separated and the aqueous layer extracted with CH2Cl2. The combined organic phases were washed successively with water, satd. NaHCO3, 0.1N HCl and satd. NaCl, dried and evaporated to dryness. The residue was treated with hexane (60 ml), and the resultant solid was collected by filtration, washed with hexane and dried to give 14.2 g (62 mmole, 63%) of the title compound as a white solid, mp 72°-3° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05585358 |
| Source dataset | uspto-grants-1996_12 |
| ORD ID | ord-4e7f39d9fabb4b3aab5f41389c7fbd48 |
| Source note | uspto-grants-1996_12 |