2-庚醇 → 1-甲基乙酸己酯

HRID 1604135

反应方程式

HRID 1604135 反应方程式
[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]

参与物

4

实验过程

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).

后处理

  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

来源与证据

ORD记录
ord-4204bf78b3bc48c3a333a66f64dc3810
来源数据集
uspto-grants-1999_11
专利号
US05993879

关联笔记

加载中…