反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 275 °C
PROCEDURE
实验过程
4770 g of isostearic acid isopropyl ester (Emery 2310 isostearic acid isopropyl ester, sold by Emery Industry Inc., U.S.A.) and 239 g of a copper-chromium catalyst (made by Nikki) are charged in an autoclave having a capacity of 20 liters. Hydrogen gas is then added under a pressure of 150 kg/cm2 and the reaction mixture is heated to a temperature of 275° C. Hydrogenation was carried out under a pressure of 150 kg/cm2 at 275° C. for about 7 hours, and then the reaction product was cooled and the catalyst residue was removed by filtration, whereupon 3500 g of a crude product were obtained. The crude product was distilled under reduced pressure thereby obtaining 3300 g of a colourless transparent isostearyl alcohol as a distillate at 80° to 167° C./0.6 mmHg. The isostearyl alcohol (methyl-branched stearyl alcohol) thus prepared had an acid value of 0.05, a saponification value of 5.5, and a hydroxyl value of 181.4. Absorption was observed at 3340 and 1055 cm-1 by IR (liquid film) and at δ3.50 (broad triplet, --CHH2 --OH) by NMR(CCl4). It has been found from gas-chromatography that the alcohol consists of a mixture which comprises about 75% of the main component having a total carbon number of 18 (the total of m and n being 15 in the formula II) and the rest being composed of components having a total carbon number of 14 or 16, and that, in any case, branched methyl groups are located in the vicinity of the center of the main alkyl chain.
WORKUP
后处理
- temperaturethe reaction product was cooled
- customthe catalyst residue was removed by filtration, whereupon 3500 g of a crude product
- customwere obtained
- distillationThe crude product was distilled under reduced pressure