HRID482942

反应详情

EQUATION

反应方程式

HRID 482942 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
275 °C

PROCEDURE

实验过程

Into a 20 liters autoclave were charged 4770 g of isopropyl isostearate [Emery 2310, commercially available from Emery Co., Ltd. U.S.A.] and 239 g of copper-chromium catalyst (product of Nikki Co., Ltd.). Hydrogen gas was charged into the reactor under a pressure of 150 kg/cm2 and the reaction mixture was heated up to 275° C. After hydrogenation under 150 kg/cm2 /275° C. for about 7 hours, the reaction product was cooled, followed by removing the catalyst residue by filtration to obtain 3500 g of crude product. The crude product was distilled under reduced pressure thereby obtaining 3300 g of colorless transparent isostearyl alcohol as a fraction of 80° to 167° C./0.6 mmHg. The thus obtained isostearyl alcohol (monomethyl-branched isostearyl alcohol) had an acid value of 0.05, a saponification value of 5.5, and a hydroxyl value of 181.4. IR analysis (liquid film) revealed absorptions at 3340 and 1055 cm-1 and NMR analysis (CCl4 solvent) revealed an absorption at (δ)=3.50 (broad triplet, --CH2 --OH). According to the gas chromatograph, the alcohol was chiefly composed of about 75% of an alcohol whose number of carbon atoms in the alkyl group was 18, with the remainder being made of alcohols having alkyl groups with 14 and 16 carbon atoms. The branched methyl group was located substantially at the center of the main alkyl chain in all the alcohol components.

WORKUP

后处理

  1. temperaturethe reaction product was cooled
  2. customby removing the catalyst residue
  3. filtrationby filtration
  4. customto obtain 3500 g of crude product
  5. distillationThe crude product was distilled under reduced pressure