Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Methyl iodide | HCID 6328 | — |
| Reactant | 2-((1,1-Dimethylethyl)imino)-N,N-diethylhexahydro-1,3-dimethyl-2lambda5-1,3,2-diazaphosphorin-2-amine | HCID 3513851 | — |
| Reactant | HCID 66614606 | HCID 66614606 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 66614348 | HCID 66614348 | 36.3% |
Reaction Steps
80 mg (0.175 mmol) of the compound from example 36 and 48 mg (0.175 mmol) of BEMP were initially charged in 10 ml of dimethylformamide, and a solution of 25 mg (0.175 mmol) of iodomethane in 2 ml of dimethylformamide was added dropwise at 0° C. within 10 min. The mixture was stirred at 0° C. for 20 min. Subsequently, the reaction solution was concentrated under reduced pressure and the residue was purified by means of preparative HPLC (eluent: methanol/water, gradient 30:70→90:10). 30 mg of the title compound were obtained (35% of theory).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US09096592B2 |
|---|
| Source dataset | uspto-grants-2015_08 |
|---|
| ORD ID | ord-e9fd92fd3a744b1abafeffd826e690b1 |
|---|
| Source note | uspto-grants-2015_08 |
|---|
