2-Heptanol → 1-Methylhexyl acetate

HRID 1604135

反応式

HRID 1604135 の反応式
[CH3:1][CH:2]([OH:8])[CH2:3][CH2:4][CH2:5][CH2:6][CH3:7].[C:9]([O-])(=[O:11])[CH3:10].[Na+]>C(OC(=O)C)(=O)C>[C:9]([O:8][CH:2]([CH3:1])[CH2:3][CH2:4][CH2:5][CH2:6][CH3:7])(=[O:11])[CH3:10]

参加物

4

反応物 2

HCID 109762-HeptanolHCID 517045Sodium Acetate

生成物 1

HCID 800181-Methylhexyl acetate収率 67%

試薬・触媒・溶媒 1

HCID 7918Acetic Anhydride溶媒

実験手順

2-Heptanol (162 g, 1.4 mol, Aldrich) and sodium acetate (16 g, Aldrich) were heated to 100° C. and then acetic anhydride (190 ml, BDH GPR) was added over a 1 hour period at 100-130° C. The mixture was heated to reflux for 3 hours. The reaction mixture was then cooled, washed with water, washed with aqueous sodium bicarbonate to neutrality, dried over sodium sulfate, and then concentrated. Fractional distillation of the crude residue under vacuum provided 1-methylhexyl acetate (107-108°/95-100 mm Hg, 67% yield), the structure of which was confirmed by mass spectroscopy, nuclear magnetic resonance spectroscopy, and infra red spectroscopy (not shown).

後処理

  1. temperatureThe mixture was heated
  2. temperatureto reflux for 3 hours
  3. temperatureThe reaction mixture was then cooled
  4. washwashed with water
  5. washwashed with aqueous sodium bicarbonate to neutrality
  6. dry with materialdried over sodium sulfate
  7. concentrationconcentrated
  8. distillationFractional distillation of the crude residue under vacuum

出典と根拠

ORDレコード
ord-4204bf78b3bc48c3a333a66f64dc3810
出典データセット
uspto-grants-1999_11
特許番号
US05993879

関連ノート

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