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 178508324 | HCID 178508324 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 66635326 | HCID 66635326 | — |
Reaction Steps
250 mg (0.692 mmol) of the compound from example 53 and 190 mg (0.692 mmol) of BEMP were initially charged in 12 ml of dimethylformamide, and a solution of 98 mg (0.692 mmol) of iodomethane in 3 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/aqueous 0.1% ammonia solution=65:35). The residue was stirred with acetonitrile and filtered with suction, and the solids were dried under high vacuum. 78 mg of the title compound (30% of theory) and 50 mg of example 55 were obtained (19% of theory).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US09096592B2 |
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| Source dataset | uspto-grants-2015_08 |
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| ORD ID | ord-05372999da4c4cf5b189bd26eadb7d10 |
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| Source note | uspto-grants-2015_08 |
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