HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 86686940, compound → HCID 86686939, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 86686940 | HCID 86686940 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 86686939 | HCID 86686939 | 73.5% |
Reaction Steps
In a 100 ml three-neck flask, said 3′,5′-dichloro-4-(trichloro methyl sulfenyl)benzophenone is added into 80 g methanol. The solution is heated with stirring under nitrogen protection to reflux for 5 h, and then is distilled to remove the methanol and all low-boiling-point substances. The residue is recrystallized in a mixed solvent consisting of ethyl acetate and petroleum ether in a weight ratio 1:1 to obtain 21 g yellow-green needle-like crystals with a purity of 98.8%, the yield is 73.5%, and the melting point is 98-99° C. 1H-NMR data (solvent CDCl3): δ3.6808 ppm, s, 1H; δ7.3431, 7.3700 ppm, d, 2H; δ7.5665, 7.5702 ppm, d, 1H; δ7.6033, 7.6065 ppm, d, 2H; 7.6489, 7.6758 ppm, d, 2H.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09409861B2 |
| Source dataset | uspto-grants-2016_08 |
| ORD ID | ord-95cf66d4b7244119ac41e03e5a993e19 |
| Source note | uspto-grants-2016_08 |