HuagongsheHuagongshe Chemistry Print Report · For research reference only
4-Chloro-2-(methylthio)pyrimidine-5-carboxylic acid ethyl ester → Ethyl 4-[2-(2-chlorophenyl)hydrazino]-2-(methylthio)pyrimidine-5-carboxylate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 4-Chloro-2-(methylthio)pyrimidine-5-carboxylic acid ethyl ester | HCID 80008 | — |
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | 2-Chlorophenylhydrazine hydrochloride | HCID 443287 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | Ethyl 4-[2-(2-chlorophenyl)hydrazino]-2-(methylthio)pyrimidine-5-carboxylate | HCID 67171554 | — |
Reaction Steps
At room temperature, 16.2 mL of N,N-diisopropylethylamine was added to tetrahydrofuran (300 mL) solution of 9.4 g of ethyl 4-chloro-2-(methylthio)pyrimidine-5-carboxylate and 8.3 g of 2-chlorophenylhydrazine hydrochloride, and heated under reflux for 18 hours. The solvent was concentrated under reduced pressure, water was added to this, and extracted with ethyl acetate, and the ethyl acetate layer was washed with saturated saline water, and dried with anhydrous sodium sulfate. The solvent was evaporated away under reduced pressure to obtain crude ethyl 4-[2-(2-chlorophenyl)hydrazino]-2-(methylthio)pyrimidine-5-carboxylate as a yellow oily substance.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07935708B2 |
| Source dataset | uspto-grants-2011_05 |
| ORD ID | ord-48d5b8a2b45f43f19f7c8741247eb5ef |
| Source note | uspto-grants-2011_05 |