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Chloroethane → HCID 13388143, 화합물

HRID 638011
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HRID 638011 반응식
[CH3:1][C:2]1[C:10]([C:11](=[O:18])[C:12]2[CH2:17][CH2:16][CH2:15][NH:14][CH:13]=2)=[C:5]2[CH:6]=[CH:7][CH:8]=[CH:9][N:4]2[N:3]=1.[H-].[Na+].[CH2:21](Cl)[CH3:22]>CN(C)C=O>[CH3:1][C:2]1[C:10]([C:11](=[O:18])[C:12]2[CH2:17][CH2:16][CH2:15][N:14]([CH2:21][CH3:22])[CH:13]=2)=[C:5]2[CH:6]=[CH:7][CH:8]=[CH:9][N:4]2[N:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 6337ChloroethaneHCID 24758Sodium hydrideHCID 146826KC 764

생성물 1

HCID 13388143HCID 13388143, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

One g of 2-methyl-3-(1,4,5,6-tetrahydronicotinoyl)pyrazolo[1,5-a]pyridine was dissolved in 20 ml of dimethyl-formamide and 0.3 g of sodium hydride (55%) was added whilst stirring to the mixture. The mixture was stirred at room temperature for 1 hour, and then 1 g of ethylchloride was added and stirred at 60° C. for 2 hours. After removal of solvent in vacuo, the residue was chromatographed over SiO2 employing CH2Cl2 --ethyl acetate--methanol (8:1.5:0.5) mixture as eluent. The eluate was evaporated to dryness in vacuo and the residue was recrystallized from benzene-hexane to afford the title compound in yield of 0.8 g (72%), mp. 104°-105° C.

후처리

  1. stirringThe mixture was stirred at room temperature for 1 hour
  2. stirringstirred at 60° C. for 2 hours
  3. customAfter removal of solvent in vacuo
  4. customthe residue was chromatographed over SiO2
  5. customThe eluate was evaporated to dryness in vacuo
  6. customthe residue was recrystallized from benzene-hexane

출처 및 근거

ORD 기록
ord-ab199b9f41e24b40bbf9899bbed7d1d3
출처 데이터셋
uspto-grants-1985_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04559402

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