HuagongsheHuagongshe Chemistry Print Report · For research reference only
Guanidine → HCID 20729541, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Guanidine | HCID 3520 | — |
| Reactant | tert-Butoxy bis(dimethylamino)methane | HCID 79885 | — |
| Reactant | HCID 20729568 | HCID 20729568 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 20729541 | HCID 20729541 | — |
Reaction Steps
To a solution of compound 6 (1 equivalent) in THF, at ambient temperature, was added (Me2N)2CHOt-Bu (3 equivalents). After 24 hours, the solvent was evaporated and the crude product was utilized without purification. Step 2: To a solution of the compound formed above at Step 1 (1 equivalent) in ethanol, at ambient temperature, was added guanidine (3 equivalents) and the resulting mixture heated at reflux. After 12 hours, the solvent was evaporated and the crude product purified by preparatory HPLC (reverse phase; 10–90% MeCN in water; 15 minutes) to afford the desired compound III-a-74. HPLC using method B provided Rt of 7.9 minutes. 1H NMR was consistent with expected structure. FIA/MS Obs. M+1/M−1.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07253187B2 |
| Source dataset | uspto-grants-2007_08 |
| ORD ID | ord-7e556ac7efbc4216850695948e8b9e4d |
| Source note | uspto-grants-2007_08 |