Isopropyl Isostearate → Isostearyl Alcohol EX

HRID 979881

반응식

HRID 979881 반응식
C([O:4][C:5](=O)[CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH:20]([CH3:22])[CH3:21])(C)C.[H][H]>[Cr].[Cu]>[CH2:5]([OH:4])[CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH:20]([CH3:21])[CH3:22]

참가 물질

4

반응물 2

HCID 94625Isopropyl IsostearateHCID 178418361HCID 178418361, 화합물

생성물 1

HCID 62825Isostearyl Alcohol EX수율 83.5%

시약·촉매·용매 1

HCID 9833946Chromium, compd. with copper (1:1)촉매

반응 조건

온도
275 °C

실험 절차

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.

후처리

  1. temperaturethe reaction product was cooled
  2. customthe catalyst residue was removed by filtration, whereupon 3500 g of a crude product
  3. customwere obtained
  4. distillationThe crude product was distilled under reduced pressure

출처 및 근거

ORD 기록
ord-ca70944ccc734fbe83ecdd385e909f4b
출처 데이터셋
uspto-grants-1987_01
특허 번호
US04634719

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