Sodium Hydroxide → HCID 178418460、化合物

HRID 3246

反応式

HRID 3246 の反応式
Cl.Cl[CH2:3][C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][N:5]=1.[CH3:10][C:11]1([CH3:18])[NH:15][C:14](=[S:16])[NH:13][C:12]1=[S:17].[OH-].[Na+]>>[N:5]1[CH:6]=[CH:7][CH:8]=[CH:9][C:4]=1[CH2:3][S:16][C:14]1[NH:15][C:11]([CH3:18])([CH3:10])[C:12](=[S:17])[N:13]=1

参加物

4

反応物 3

HCID 14798Sodium HydroxideHCID 23392Picolyl chloride hydrochlorideHCID 30021425,5-Dimethyl-2,4-imidazolidinedithione

生成物 1

HCID 178418460HCID 178418460、化合物

実験手順

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%.

後処理

  1. extractionextracted with 100 mL of chloroform (CHCl3)
  2. dry with materialThe CHCl3 layer was dried over MgSO4
  3. concentrationconcentrated in vacuo
  4. customThe residue was purified by column chromatography (
  5. customAs a result, 2-(2-pyridylmethylthio) was initially obtained

出典と根拠

ORDレコード
ord-dc25bdb7c4ad482f819d561626b78d70
出典データセット
uspto-grants-1998_03
特許番号
US05733922

関連ノート

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