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Oxygen → 3-ethyl-2,4-pentanediol Dibenzoate

HRID 132720
ノート
印刷プレビュー

反応式

HRID 132720 の反応式
O=O.[CH2:3]([CH:5]([CH:9]([OH:11])[CH3:10])[CH:6]([OH:8])[CH3:7])[CH3:4].N1C=C[CH:15]=[CH:14][CH:13]=1.[C:18](Cl)(=[O:25])[C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1.[CH2:27]1[CH2:31][O:30][CH2:29][CH2:28]1>N#N.O>[C:18]([O:8][CH:6]([CH:5]([CH2:3][CH3:4])[CH:9]([O:11][C:29](=[O:30])[C:28]1[CH:27]=[CH:31][CH:15]=[CH:14][CH:13]=1)[CH3:10])[CH3:7])(=[O:25])[C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 5

HCID 977OxygenHCID 1049PyridineHCID 7412Benzoyl chlorideHCID 8028TetrahydrofuranHCID 218678653-Ethyl-2,4-pentanediol

生成物 1

HCID 231259023-ethyl-2,4-pentanediol Dibenzoate

試薬・触媒・溶媒 2

HCID 947
Nitrogen
溶媒
HCID 962Water溶媒

実験手順

In N2 atmosphere free of water and oxygen, to a reactor were successively added 0.02 mol 3-ethyl-2,4-pentanediol, 20 ml THF, and 0.06 mol pyridine, then slowly added dropwise 0.05 mol benzoyl chloride. The reaction was heated refluxing for 8 hours, and allowed to continue at room temperature for further 12 hours. After the reaction was finished, the reaction mixture was filtered and the cake was washed with anhydrous ethyl ether for three times. The organic phase was completely washed with saturated saline, and dried over anhydrous sodium sulfate. Removing the solvent gave 5.1 g product.

後処理

  1. temperatureThe reaction was heated
  2. temperaturerefluxing for 8 hours
  3. filtrationthe reaction mixture was filtered
  4. washthe cake was washed with anhydrous ethyl ether for three times
  5. washThe organic phase was completely washed with saturated saline
  6. dry with materialdried over anhydrous sodium sulfate
  7. customRemoving the solvent

出典と根拠

ORDレコード
ord-8f2f5528e6f94937a17744271aec00d2
出典データセット
uspto-grants-2008_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07388061B2

反応ノート

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