HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triphenylphosphine → HCID 22036430, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triphenylphosphine | HCID 11776 | — |
| Reactant | 2,1,3-Benzothiadiazol-4-ol | HCID 4914673 | — |
| Reactant | Diethyl azodicarboxylate | HCID 5462977 | — |
| Reactant | 2-[3-(4-Tert-butoxycarbonyl-1-piperazinyl)-2-pyrazinyloxy]ethanol | HCID 11416074 | — |
| Product | HCID 22036430 | HCID 22036430 | 12% |
Reaction Steps
DEAD (0.52 mL, 3.3 mmol) was added to a slurry of 2-[3-(4-tert-butoxycarbonyl-1-piperazinyl)-2-pyrazinyloxy]ethanol (1.00 g, 3.08 mmol; prepared in Example 52, Step 2), 4-hydroxy-2,1,3-benzothiadiazole*(0.46 g, 3.0 mmol) and resin bound PPh3 (1.1 g, 3.3 mmol) and shaken until HPLC showed no starting material. The mixture was filtered to remove the resin, concentrated and purified by column chromatography on silica to give 0.163 g (12%) of the title compound. Pos-EI-MS shows M+ and 11 ions supporting the stated structure. HRMS m/z calcd for C21H26N6O4S (M)+458.1736, found 458.1716.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07071180B2 |
| Source dataset | uspto-grants-2006_07 |
| ORD ID | ord-76743798522c4873b8d0ec064b4b88d7 |
| Source note | uspto-grants-2006_07 |