HuagongsheHuagongshe Chemistry Print Report · For research reference only
2,2,2-Trifluoroethyl trichloromethanesulphonate → HCID 66614119, 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 178508323 | HCID 178508323 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 66614119 | HCID 66614119 | 45% |
Reaction Steps
100 mg (0.278 mmol) of the compound from example 58 and 76 mg (0.278 mmol) of BEMP were initially charged in 3 ml of dimethylformamide, a solution of 78 mg (0.266 mmol) of 2,2,2-trifluoroethyl trichloromethanesulfonate in 2 ml of dimethylformamide was added dropwise at 0° C. within 10 min and the mixture was stirred at RT for 20 min The product was precipitated by adding water, filtered off with suction and purified by means of preparative HPLC (eluent: acetonitrile/water with 0.05% trifluoroacetic acid, gradient 20:80→50:50). 53 mg of the title compound were obtained (43% of theory).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09096592B2 |
| Source dataset | uspto-grants-2015_08 |
| ORD ID | ord-ff5868d529ce4bd59ada21b43155b1b4 |
| Source note | uspto-grants-2015_08 |