Carbon Disulfide → triethylammonium N-(2-pyrazinyl)-dithiocarbamate

HRID 51982ノート

反応式

HRID 51982 の反応式
[NH2:1][C:2]1[CH:3]=[N:4][CH:5]=[CH:6][N:7]=1.[C:8](=[S:10])=[S:9].C(OCC)(=O)C.[CH2:17]([N:19]([CH2:22][CH3:23])[CH2:20][CH3:21])[CH3:18]>CCCCCC>[N:7]1[CH:6]=[CH:5][N:4]=[CH:3][C:2]=1[NH:1][C:8](=[S:9])[S-:10].[CH2:17]([NH+:19]([CH2:22][CH3:23])[CH2:20][CH3:21])[CH3:18]

参加物

6

反応物 4

HCID 6348Carbon DisulfideHCID 8471TriethylamineHCID 8857Ethyl AcetateHCID 78747Aminopyrazine

生成物 1

HCID 19962701triethylammonium N-(2-pyrazinyl)-dithiocarbamate収率 31.6%

試薬・触媒・溶媒 1

HCID 8058Hexane溶媒

実験手順

In a 100-ml flask, 4.9 g (50 mmol) of 3-aminopyrazine, 4.5 g (59 mmol) of carbon disulfide and 50 ml of ethyl acetate were placed, and 6.5 g (64 mmol) of triethylamine was added dropwise with stirring over a 5-min period on a water bath. After the mixture was stirred at 60° C. for 5 hr. 10 ml of hexane was added to the mixture, which was allowed to stand overnight at room temperature to precipitate yellow crystals. The crystals were separated from the solution by filtration, and washed with 5 ml of ethyl acetate to obtain 4.3 g of triethylammonium N-(2-pyrazinyl)-dithiocarbamate (Intermediate II-1). Yield 31%. Mp 113°-116° C. (dec).

後処理

  1. stirringAfter the mixture was stirred at 60° C. for 5 hr
  2. customto precipitate yellow crystals
  3. customThe crystals were separated from the solution by filtration
  4. washwashed with 5 ml of ethyl acetate

出典と根拠

ORDレコード
ord-44ea6459c73449988937bfaeef87df1a
出典データセット
uspto-grants-1997_04
特許番号
US05616456

反応ノート

読み込み中…