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

HRID 259380

반응식

HRID 259380 반응식
[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]

참가 물질

6

반응물 4

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

생성물 1

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

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-d786c996b26840b6a7aeeb62ddc1c96d
출처 데이터셋
uspto-grants-1977_07
특허 번호
US04038065

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