Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Water | HCID 962 | — |
| Reactant | 4-Methylmorpholine | HCID 7972 | — |
| Reactant | Phenyl chloroformate | HCID 15891 | — |
| Reactant | HCID 22866846 | HCID 22866846 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 54051803 | HCID 54051803 | 54.7% |
Reaction Steps
0.5 g of N-methylmorpholine, and subsequently 0.8 g of phenyl chloroformate were added to a suspension containing 1.4 g of N1 -[2-(4-cyanophenoxy)-1-methylethyl]-L-norvalinamide suspended in 40 ml of methylene chloride at -15° C. The mixture was allowed to sit and warm naturally to room temperature and stirred for 15 hours at room temperature. Water was subsequently added to the reaction mixture. After the methylene chloride layer was washed with water, the organic layer was dried over anhydrous magnesium sulfate and then the methylene chloride was removed under reduced pressure. The residue was purified by column chromatography on silica gel, thus obtaining 1.1 g of the desired product in the form of a colorless plated crystal (yield: 57%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US05574064 |
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| Source dataset | uspto-grants-1996_11 |
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| ORD ID | ord-dcd5a06223eb4c3d8f94e25b436c469d |
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| Source note | uspto-grants-1996_11 |
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