HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethylmorpholine → HCID 21344943, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethylmorpholine | HCID 7525 | — |
| Reactant | Butylamine | HCID 8007 | — |
| Reactant | Isobutyl chloroformate | HCID 62365 | — |
| Reactant | HCID 11044788 | HCID 11044788 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 21344943 | HCID 21344943 | — |
Reaction Steps
2.42 g of 1-(N-(tert-butoxycarbonyl)-2(S)-aminobutyryl)-L-proline (8.05 mmol) prepared as in Example 2 c) are dissolved in dry tetrahydrofuran (15 ml). The solution is cooled in an ice/salt bath and 0.927 g of N-ethylmorpholine (8.05 mmol) and 1.10 g of isobutyl chloroformate (8.05 mmol) are then added. The solution is stirred for 45 minutes and 0.59 g (8.05 mmol) of n-butylamine is added. After stirring overnight, methylene chloride (200 ml) is added and the mixture is washed with 10% citric acid (2×100 ml) and then with 5% NaHCO3 (2×100 ml). The organic phase is dried (Na2SO4) and evaporated under vacuum. A syrup is obtained. The deprotection is carried out without characterization.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06403561B1 |
| Source dataset | uspto-grants-2002_06 |
| ORD ID | ord-8e3c4f0b6eea4456bf6597573880ca32 |
| Source note | uspto-grants-2002_06 |