HuagongsheHuagongshe Chemistry Print Report · For research reference only
4-Methylmorpholine → HCID 68710374, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 4-Methylmorpholine | HCID 7972 | — |
| Reactant | Diethylamine | HCID 8021 | — |
| Reactant | Isobutyl chloroformate | HCID 62365 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | HCID 54276808 | HCID 54276808 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 68710374 | HCID 68710374 | — |
Reaction Steps
Isobutyl chloroformate (0.84 ml; 6.5 mmol) was added to a stirred solution of 4-methylmorpholine (0.72 ml; 6.5 mmol) and the compound of example 1f (2.0 g; 6.5 mmol) in DMF (10 ml) at −25° C., followed by the addition of diethyl amine (0.88 ml; 8.45 mmol). The reaction mixture was stirred for 15 min., poured into a 10% aqueous NaHCO3 solution and extracted with EtOAc. The EtOAc layer was washed with brine, concentrated and crystallized using EtOAc-PE60-80° C. to obtain the title compound. Yield, 1.95 g (82%); mp, 100-01° C.; MS (EI): 364 (M+), 291, 234 (100%); analysis: C19H28N2O5 requires C, 62.62; H, 7.74; N, 7.69; found: C, 62.43; H, 7.60; N, 7.25%.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07759387B2 |
| Source dataset | uspto-grants-2010_07 |
| ORD ID | ord-be14e40716a5401b8605225e28ec9bcb |
| Source note | uspto-grants-2010_07 |