2-Heptanol → 1-Methylhexyl acetate

HRID 1604135

반응식

HRID 1604135 반응식
[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]

참가 물질

4

반응물 2

HCID 109762-HeptanolHCID 517045Sodium Acetate

생성물 1

HCID 800181-Methylhexyl acetate수율 67%

시약·촉매·용매 1

HCID 7918Acetic Anhydride용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-4204bf78b3bc48c3a333a66f64dc3810
출처 데이터셋
uspto-grants-1999_11
특허 번호
US05993879

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