HuagongsheHuagongshe Chemistry Print Report · For research reference only
4,6-Dichloro-2-(methylthio)pyrimidine → HCID 20539481, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 4,6-Dichloro-2-(methylthio)pyrimidine | HCID 80531 | — |
| Reactant | Phosphinous acid, dicyclohexyl-, methyl ester | HCID 6931439 | — |
| Solvent | 1,2-Dichlorobenzene | HCID 7239 | — |
| Product | HCID 20539481 | HCID 20539481 | 5.3% |
Reaction Steps
A mixture of 2.50 g of methyl dicyclohexylphosphinite and 1.00 g of 4,6-dichloro-2-methylthiopyrimidine in 20 ml of o-dichlorobenzene was refluxed under nitrogen for 6.5 hours. Volatiles were removed from the mixture under vacuum, and the resulting oily residue was recrystallized twice from cyclohexane with decolorizing charcoal treatment and dried at 100° C./0.1 mm (13 Pa) to give 0.15 g of 4,6-bis(dicyclohexylphosphinyl)-2-methylthiopyrimidine (shown by formula in Claim 11) as white crystals, mp 197°-198.5° C. Anal. Calcd for C29H48N2O2P2S: C, 63.25; H, 8.79; N, 5.07; S, 5.82. Found: C, 63.19; H, 8.81; N, 4.89; S, 6.04.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04234729 |
| Source dataset | uspto-grants-1980_11 |
| ORD ID | ord-d8e70429cd784a9892318e10a17d9c3b |
| Source note | uspto-grants-1980_11 |