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Pyridine → 3-Methylnonan-3-YL-benzoate

HRID 1863146
ノート
印刷プレビュー

反応式

HRID 1863146 の反応式
[CH3:1][C:2]([OH:11])([CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH3:10])[CH2:3][CH3:4].N1C=CC=CC=1.[C:18](Cl)(=[O:25])[C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1>C1(C)C=CC=CC=1>[CH3:1][C:2]([O:11][C:18](=[O:25])[C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1)([CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH3:10])[CH2:3][CH3:4]
参加物反応条件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 1049PyridineHCID 7412Benzoyl chlorideHCID 894283-Nonanol, 3-methyl-

生成物 1

HCID 203921353-Methylnonan-3-YL-benzoate

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒2 回

反応条件

温度
5 °C

実験手順

40.0 G. (0.25 mole) of 3-methylnonan-3-ol, 20. g. of pyridine and 60 ml. of toluene are combined and cooled to 5° C. under agitation. To the resulting solutin is added, under agitation, over a period of 1 to 2 hours while maintaining the reaction temperature between 5°-15° C., a solution of 35.15 g. (0.25 mole) of benzoyl chloride, dissolved in 30 ml. of toluene. The source of cooling is removed and the reaction mixture is agitated overnight, permitting the temperature of the reaction mixture to rise to room temperature (25°-30° C.). After completion of the reaction, the formed pyridine hydrochloride is removed by successive washings with 100 ml. of warm water. The solvent is removed by distillation and the desired ester is rectified by fractional distillation in a vacuum, preferably at 1 mm.

後処理

  1. additionTo the resulting solutin is added, under agitation, over a period of 1 to 2 hours
  2. temperaturewhile maintaining the reaction temperature between 5°-15° C.
  3. temperatureThe source of cooling
  4. customis removed
  5. customto rise to room temperature
  6. custom(25°-30° C.)
  7. customAfter completion of the reaction
  8. customthe formed pyridine hydrochloride is removed by successive washings with 100 ml
  9. customThe solvent is removed by distillation
  10. distillationthe desired ester is rectified by fractional distillation in a vacuum, preferably at 1 mm

出典と根拠

ORDレコード
ord-4f33228a264d4b45b05956e1b9951530
出典データセット
uspto-grants-1979_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04168248

反応ノート

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