Ethanol → HCID 178430570, 화합물

HRID 59052

반응식

HRID 59052 반응식
Cl[C:2]1[CH:7]=[N:6][CH:5]=[C:4]([CH3:8])[N:3]=1.[O-]S(OOS([O-])(=O)=O)(=O)=O.[K+].[K+].C(O)C.[OH-:24].[Ca+2].[OH-:26]>S(=O)(=O)(O)O.C(O)C.O1CCCC1>[CH3:8][C:4]1[CH:5]=[N:6][CH:7]=[C:2]([OH:26])[N+:3]=1[O-:24]

참가 물질

7

반응물 4

HCID 702EthanolHCID 24412Potassium PersulfateHCID 6093208Calcium HydroxideHCID 71700952-Chloro-6-methylpyrazine

생성물 1

HCID 178430570HCID 178430570, 화합물

시약·촉매·용매 2

HCID 1118Sulfuric Acid용매HCID 21873804Tetrahydrofuran ethanol용매

실험 절차

156 mmol (20 g) 2-chloro-6-methylpyrazine were dissolved in 80 ml 96% sulfuric acid, 222 mmol (63 g) potassium peroxodisulfate were added portion wise at 10° C. and stirring was carried out for 2 days at 10° C. and 1 day at room temperature (see also C. E. Mixan, R. Garth, J. Org. Chem. 1977, 42, 1869-1871). The reaction mixture was poured on 200 g ice, under addition of ethanol neutralization was carried out with calcium hydroxide, then filtered off and washed with ethanol. The filtrate was evaporated until dryness, the obtained solid (20 g) were refluxed in 300 ml 20% KOH solution for 3 h and after cooling pH 3 was adjusted with 20% HCl. The solution was evaporated until dryness, the residue boiled with 0.2 l ethanol under reflux for 2 h, after cooling filtered and the filtrate evaporated until dryness. After recrystallization from ethanol/tetrahydrofuran from 7.4 g raw product 2.17 g (10% yield, 93% purity) of the title compound were obtained.

후처리

  1. filtrationfiltered off
  2. washwashed with ethanol
  3. customThe filtrate was evaporated until dryness
  4. temperaturethe obtained solid (20 g) were refluxed in 300 ml 20% KOH solution for 3 h
  5. temperatureafter cooling pH 3
  6. customThe solution was evaporated until dryness
  7. temperatureunder reflux for 2 h
  8. temperatureafter cooling
  9. filtrationfiltered
  10. customthe filtrate evaporated until dryness

출처 및 근거

ORD 기록
ord-f60c1ed51524439d8461308a086b08dd
출처 데이터셋
uspto-grants-2016_09
특허 번호
US09439910B2

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