HuagongsheHuagongshe Chemistry Print Report · For research reference only
(4-(Hydroxymethyl)phenyl)(phenyl)methanone → HCID 68506179, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | (4-(Hydroxymethyl)phenyl)(phenyl)methanone | HCID 13149642 | — |
| Reactant | Tributyltin methoxide | HCID 16683411 | — |
| Solvent | 1,2-Dichloroethane | HCID 11 | — |
| Product | HCID 68506179 | HCID 68506179 | 56.2% |
Reaction Steps
In a 50 ml dry three-neck-flask, 2.5 g (7.8 mmol) of tri-n-butylmethoxy tin are added to 1.5 g (7.1 mmol) of 4-(hydroxymethyl)-benzophenone in 15 ml of 1,2-dichlorethane at room temperature in the course of 0.5 h under argon. 1H-NMR-spectrum confirms the complete conversion. The solution is concentrated and the crude product, 3.6 g of a yellow oil, is distilled in a bulb-to-bulb distillation apparatus in vacuum (0.016 mbar) at 160-170° C. The resulting colorless oil (2.8 g) is distilled a second time in a bulb-to-bulb distillation apparatus (0.020 mbar). 2.0 g of the title product are obtained as a colorless oil (boiling area 294-308° C.). The structure is further confirmed by 1H-NMR and 13C-NMR-spectra.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08318830B2 |
| Source dataset | uspto-grants-2012_11 |
| ORD ID | ord-15cee02d21e247cd9dd3c0f2916c717f |
| Source note | uspto-grants-2012_11 |