Propylethinylcarbinol → HCID 10889347、化合物

HRID 345177

反応式

HRID 345177 の反応式
[CH:1](=[N:8][OH:9])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[CH:10]#[C:11][CH:12]([OH:16])[CH2:13][CH2:14][CH3:15].Cl[O-].[Na+]>ClCCl>[OH:16][CH:12]([C:11]1[O:9][N:8]=[C:1]([C:2]2[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=2)[CH:10]=1)[CH2:13][CH2:14][CH3:15]

参加物

5

反応物 3

HCID 7746PropylethinylcarbinolHCID 12143(Z)-Benzaldehyde oximeHCID 23665760Sodium Hypochlorite

生成物 1

HCID 10889347HCID 10889347、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

In 25 ml of dichloromethane, were dissolved 5.0 g (41.3 mmol) of benzaldoxime and 4.5 g (45.9 mmol) of 1-hexyne-3-ol. Under ice cooling, 29.0 g of a 12.0% aqueous solution of sodium hypochlorite were added dropwise to the solution over 30 minutes. After completion of the dropwise addition, they were reacted at 20° C. for 2 hours. After completion of the reaction, the reaction mixture was extracted with dichloromethane and the organic layer was washed with water. The organic layer was dried over anhydrous sodium sulfate and the solvent was then distilled off under reduced pressure. The residue was purified by chromatography on a silica gel column (eluent: chloroform), whereby the target compound, namely, 5-(1-hydroxybutyl)-3-phenylisooxazole was obtained as an oil.

後処理

  1. additionAfter completion of the dropwise addition, they
  2. customwere reacted at 20° C. for 2 hours
  3. customAfter completion of the reaction
  4. extractionthe reaction mixture was extracted with dichloromethane
  5. washthe organic layer was washed with water
  6. dry with materialThe organic layer was dried over anhydrous sodium sulfate
  7. distillationthe solvent was then distilled off under reduced pressure
  8. customThe residue was purified by chromatography on a silica gel column (eluent: chloroform), whereby the target compound

出典と根拠

ORDレコード
ord-f53c369c59d54fdfaaae38de21666242
出典データセット
uspto-grants-1991_10
特許番号
US05055585

関連ノート

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