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

HRID 51982노트

반응식

HRID 51982 반응식
[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]

참가 물질

6

반응물 4

HCID 6348Carbon DisulfideHCID 8471TriethylamineHCID 8857Ethyl AcetateHCID 78747Aminopyrazine

생성물 1

HCID 19962701triethylammonium N-(2-pyrazinyl)-dithiocarbamate수율 31.6%

시약·촉매·용매 1

HCID 8058Hexane용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-44ea6459c73449988937bfaeef87df1a
출처 데이터셋
uspto-grants-1997_04
특허 번호
US05616456

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