반응 #3342

반응 방정식

2-chloromethylpyridine hydrochloride

5,5-dimethyl-2,4-dithiohydantoin

NaOH

→

2-(2-pyridylmethylthio)-5,5-dimethylimidazolin-4-thione

반응 조건

후처리

1. 1
   추출extracted with 100 mL of chloroform (CHCl3)
2. 2
   건조The CHCl3 layer was dried over MgSO4
3. 3
   농축concentrated in vacuo
4. 4
   기타The residue was purified by column chromatography (
5. 5
   기타As a result, 2-(2-pyridylmethylthio) was initially obtained

실험 절차

Initially, 2.7 g of 2-chloromethylpyridine hydrochloride was added to a solution of 2.4g of 5,5-dimethyl-2,4-dithiohydantoin in 17 mL of 2N aqueous solution of NaOH. The reaction mixture was stirred for one hour at the room temperature, and extracted with 100 mL of chloroform (CHCl3). The CHCl3 layer was dried over MgSO4 and concentrated in vacuo. The residue was purified by column chromatography (using CHCl3 as a developing solvent). As a result, 2-(2-pyridylmethylthio) was initially obtained. From the earlier fractions, the desired compound of 2-(2-pyridylmethylthio)-5,5-dimethylimidazolin-4-thione was isolated in the form of a syrup. The yield of this compound was 1.02 g with a yield ratio of 27.1%.

출처