Sodium Hydroxide → 2-(2-Dimethylaminoethylamino)-5,6-dimethyl pyrazine

HRID 614310노트

반응식

HRID 614310 반응식
Cl[C:2]1[CH:7]=[N:6][C:5]([CH3:8])=[C:4]([CH3:9])[N:3]=1.[CH3:10][N:11]([CH2:13][CH2:14][NH2:15])[CH3:12].[OH-].[Na+]>O>[CH3:10][N:11]([CH3:12])[CH2:13][CH2:14][NH:15][C:2]1[CH:7]=[N:6][C:5]([CH3:8])=[C:4]([CH3:9])[N:3]=1

참가 물질

5

반응물 3

HCID 14798Sodium HydroxideHCID 66053N,N-DimethylethylenediamineHCID 126003905-Chloro-2,3-dimethylpyrazine

생성물 1

HCID 233499152-(2-Dimethylaminoethylamino)-5,6-dimethyl pyrazine

시약·촉매·용매 1

HCID 962Water용매

실험 절차

2-chloro-5,6-dimethylpyrazine (12.8 g., 0.09 mole) is added to unsym-dimethylethylenediamine (26 g., 0.295 mole) containing cuprous chloride (0.25 g.) and the mixture is heated for 48 hours in an oil bath maintained at 135°-140° C. On cooling, 50 ml of water and a single molar excess of 10N sodium hydroxide are added. The mixture is extracted with methylene chloride. The organic extracts are backwashed with saturated sodium chloride solution, dried over sodium sulfate, filtered and concentrated under vacuum. The residual oil is dissolved in hexane, filtered and reconcentrated to obtain the product oil (15.8 g., 0.081 mole).

후처리

  1. temperaturethe mixture is heated for 48 hours in an oil bath
  2. temperaturemaintained at 135°-140° C
  3. temperatureOn cooling
  4. extractionThe mixture is extracted with methylene chloride
  5. dry with materialdried over sodium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated under vacuum
  8. dissolutionThe residual oil is dissolved in hexane
  9. filtrationfiltered
  10. customto obtain the product oil (15.8 g., 0.081 mole)

출처 및 근거

ORD 기록
ord-717317f935e04e23a2f7aa78fd13bba6
출처 데이터셋
uspto-grants-1979_03
특허 번호
US04144338

반응 노트

불러오는 중…