Octane → 1-(2-Ethylhexyl)-3-cyano-6-methylpyrid-2-one

HRID 259380

反応式

HRID 259380 の反応式
[CH2:1]([CH:3]([CH2:11][CH2:12][CH2:13][CH3:14])[CH2:4][NH:5][C:6](=[O:10])[CH2:7][C:8]#[N:9])[CH3:2].CO[CH:17]=[CH:18][C:19](=O)[CH3:20].COCCO.CCCCCCCC>C(Cl)Cl>[CH2:1]([CH:3]([CH2:11][CH2:12][CH2:13][CH3:14])[CH2:4][N:5]1[C:19]([CH3:20])=[CH:18][CH:17]=[C:7]([C:8]#[N:9])[C:6]1=[O:10])[CH3:2]

参加物

6

反応物 4

HCID 356OctaneHCID 80192-MethoxyethanolHCID 942973-Buten-2-one, 4-methoxy-2 回HCID 45907042-cyano-N-(2-ethylhexyl)acetamide

生成物 1

HCID 203121811-(2-Ethylhexyl)-3-cyano-6-methylpyrid-2-one収率 90%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

N-(2-ethylhexyl) cyanoacetamide (60.4 g., 0.30 mole), 4-methoxy-3-butene-2-one (60.0 g., 0.60 mole), methylcello-solve (250 ml.) and 1,4-diazobicyclo [2.2.2.] octane (6.0 g.) are heated at reflux for 4 hours. Additional 4-methoxy-3-butene-2-one (30 g.) is added and reflux is continued for another 2 hours. The solvent is removed in vacuo to give an oil. The oil is dissolved in methylene chloride and extracted first with 2N--HCl (150 ml.) and then with water (2 × 250 ml.). The organic layer is dried over sodium sulfate, filtered and evaporated to dryness to give a 90% yield of crude product which is characterized by nmr and ir analysis.

後処理

  1. temperatureat reflux for 4 hours
  2. temperaturereflux
  3. customThe solvent is removed in vacuo
  4. customto give an oil
  5. extractionextracted first with 2N
  6. dry with materialThe organic layer is dried over sodium sulfate
  7. filtrationfiltered
  8. customevaporated to dryness

出典と根拠

ORDレコード
ord-d786c996b26840b6a7aeeb62ddc1c96d
出典データセット
uspto-grants-1977_07
特許番号
US04038065

関連ノート

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