HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 86720057, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Triethylsilane | HCID 12052 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | HCID 86720058 | HCID 86720058 | — |
| Solvent | Trifluoroacetic acid | HCID 6422 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 86720057 | HCID 86720057 | 85.1% |
Reaction Steps
471 mg (0.60 mmol) of the compound from example 85A were dissolved in 15 ml of trifluoroacetic acid, 698 mg (6.01 mmol) of triethylsilane were added and the mixture was heated to reflux for 18 h. The reaction mixture was admixed with water and ethyl acetate, and neutralized with saturated aqueous sodium hydrogencarbonate solution. The organic phase was dried over sodium sulfate and concentrated on a rotary evaporator. The residue was dried under high vacuum, and purified by means of preparative HPLC (eluent: methanol/water with 0.1% trifluoroacetic acid, gradient 30:70→90:10). 252 mg of the title compound were obtained (85% of theory).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09096592B2 |
| Source dataset | uspto-grants-2015_08 |
| ORD ID | ord-33b9055b3ec145669411762c9de5a9d2 |
| Source note | uspto-grants-2015_08 |