Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Prenderol | HCID 8284 | — |
| Reactant | Dicyclohexylcarbodiimide | HCID 10868 | — |
| Reactant | N-Carbobenzoxy-L-valine | HCID 726987 | — |
| Catalyst | 4-(Dimethylamino)pyridine | HCID 14284 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 53986985 | HCID 53986985 | — |
Reaction Steps
To a cooled solution of 2-ethyl-2-hydroxymethyl-butan-1-ol (33.1 g, 250 mmole), 4-dimethylaminopyridine (1.22 g, 10 mmole) and N-benzyloxycarbonyl-L-valine (12.6 g, 50 mmole) in 350 ml dichloromethane was added dropwise a solution of dicyclohexyl-carbodiimide (12.4 g, 60 mmole) in 50 ml dichloromethane. The mixture was stirred 2 days at room temperature and cooled. The urethane was filtered and the solution evaporated under reduced pressure. 350 ml ethyl acetate was added and the organic phase was washed twice with 5% acetic acid, 5% sodium-hydrogencarbonate and water. The organic phase was dried with sodium sulfat and evaporated under reduced pressure. The product was isolated by silica gel column chromatography with dichloromethane/methanol. Yield: 16.4 g=90%.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US07071173B2 |
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| Source dataset | uspto-grants-2006_07 |
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| ORD ID | ord-148fd3d2081f40a0ab81c04f4766a0e1 |
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| Source note | uspto-grants-2006_07 |
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