HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → DL-5 Chloro-4-(alpha-ethyl-3-phenoxybenzylamino)-6-methylthiomethylpyrimidine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Toluene | HCID 1140 | — |
| Reactant | Methylmercaptan sodium | HCID 45051789 | — |
| Reactant | DL-5 Chloro-6-chloromethyl-4-(alpha-ethyl-3-phenoxybenzyl)aminopyrimidine | HCID 131716257 | — |
| Solvent | Methanol | HCID 887 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | DL-5 Chloro-4-(alpha-ethyl-3-phenoxybenzylamino)-6-methylthiomethylpyrimidine | HCID 131716255 | — |
Reaction Steps
To a solution of 2.0 g of dl-5-chloro-6-chloromethyl-4-(α-ethyl-3-phenoxybenzyl)aminopyrimidine obtained in Example 4 dissolved in 50 ml of methanol was added 10 ml of a 15% aqueous methanthiol sodium salt solution, and the mixture was refluxed under stirring for 2 hours. After completion of the reaction, the product was poured into water and extracted with ethyl acetate. The extract was washed with water, dried over anhydrous sodium sulfate and the solvent was distilled off under reduced pressure. The oily product obtained was isolated by chromatography (Wako Gel C-200, trade name, eluted with toluene:ethyl acetate=5:1) to give 1.8 g of the desired product as pale yellow oily liquid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04895849 |
| Source dataset | uspto-grants-1990_01 |
| ORD ID | ord-5e85b2df28114c38ad359e28446850a2 |
| Source note | uspto-grants-1990_01 |