HuagongsheHuagongshe Chemistry Print Report · For research reference only
4-Methylmorpholine → HCID 86646545, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 4-Methylmorpholine | HCID 7972 | — |
| Reactant | O-(Benzotriazol-1-yl)-N,N,N',N'-tetramethyluronium tetrafluoroborate | HCID 2733207 | — |
| Reactant | HCID 86646547 | HCID 86646547 | — |
| Reactant | HCID 86646548 | HCID 86646548 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 86646545 | HCID 86646545 | — |
Reaction Steps
OO7, 4-cyclopentyl-3-oxopiperazin-1-ium trifluoroacetate (1 eq.), TBTU (1 eq.) and N-methyl-morpholine (2.2 eq.) were stirred for 2 h in DMF. The product was purified by preparative HPLC (water/MeCN, 0.1% TFA as eluents) and desired pooled product fractions were lyophilized to afford a white powder. The powder was dissolved in DCM and washed with sat. aq. NaHCO3. The organic phase was dried (Na2SO4), filtered and concentrated to dryness to afford the product as colourless oil. 1H-NMR (300 MHz, DMSO-d6) δ: 13.52 (1H, s), 7.90 (1H, s), 7.46-7.22 (3H, m), 4.82-4.65 (1H, m), 4.15 (1H, s), 4.03 (2H, s), 3.80 (2H, s), 3.42-3.20 (3H, m), 1.80-1.40 (8H, m). MS (ES) C23H22F6N4O3 requires: 516, found: 517 (M+H)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08268827B2 |
| Source dataset | uspto-grants-2012_09 |
| ORD ID | ord-a4965a971ebf42b4867ff04fe4cc7101 |
| Source note | uspto-grants-2012_09 |