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Chloroethane → HCID 13388143、化合物

HRID 638011
ノート
印刷プレビュー

反応式

HRID 638011 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 6337ChloroethaneHCID 24758Sodium hydrideHCID 146826KC 764

生成物 1

HCID 13388143HCID 13388143、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-ab199b9f41e24b40bbf9899bbed7d1d3
出典データセット
uspto-grants-1985_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04559402

反応ノート

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