HuagongsheHuagongshe Chemistry Print Report · For research reference only
2,2,2-Trifluoroethyl trichloromethanesulphonate → HCID 56928840, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 2,2,2-Trifluoroethyl trichloromethanesulphonate | HCID 90027 | — |
| 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 56928840 | HCID 56928840 | 12% |
Reaction Steps
150 mg (0.415 mmol) of the compound from example 53 and 113 mg (0.0415 mmol) of BEMP were initially charged in 7 ml of dimethylformamide, and a solution of 117 mg (0.415 mmol) of 2,2,2-trifluoroethyl trichloromethanesulfonate in 2.5 ml of dimethylformamide was added dropwise at 0° C. within 10 min. The mixture was stirred at RT for 16 h. Subsequently, the reaction solution was concentrated under reduced pressure and the residue was purified by means of preparative HPLC (eluent: acetonitrile/water with 0.05% trifluoroacetic acid, gradient 10:90→90:10). 22 mg of the title compound were obtained (11% of theory).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09096592B2 |
| Source dataset | uspto-grants-2015_08 |
| ORD ID | ord-6a212df274df442da88306cd6b7aea03 |
| Source note | uspto-grants-2015_08 |