1,2-Octadecanediol → Pentadecanediol Octadecanediol

HRID 371370

Reaktionsgleichung

Reaktionsgleichung von HRID 371370
[CH2:1]([OH:17])[CH:2]([OH:16])[CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH3:15].C(O)C([OH:34])CCCCCCCCCCCCCC.C(O)C(O)CCCCCCCCCCCCCCC.[CH2:55]([OH:74])[CH:56](O)[CH2:57][CH2:58][CH2:59][CH2:60][CH2:61][CH2:62][CH2:63][CH2:64][CH2:65][CH2:66][CH2:67][CH2:68][CH2:69][CH2:70][CH2:71][CH3:72].P(O)(OC)OC>CO>[CH:1]([OH:17])([OH:34])[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][CH2:13][CH2:14][CH3:15].[CH:55]([OH:74])([OH:16])[CH2:56][CH2:57][CH2:58][CH2:59][CH2:60][CH2:61][CH2:62][CH2:63][CH2:64][CH2:65][CH2:66][CH2:67][CH2:68][CH2:69][CH2:70][CH2:71][CH3:72]

Komponenten

7

Edukt 5

HCID 893141,2-OctadecanediolHCID 94853Dimethyl ester phosphorous acidHCID 980371,2-HexadecanediolHCID 118123Pentadecane-1,2-diolHCID 30157061,2-Heptadecanediol

Produkt 1

HCID 86740139Pentadecanediol Octadecanediol

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Reaktionsbedingungen

Temperatur
70 °C

Versuchsvorschrift

Approximately 360 g of the 1,2-mixed pentadecanedioloctadecanediol (obtained from Viking Chemical Co. as Vikol 158 containing about 28% 1,2-pentadecanediol, about 28% 1,2-hexadecanediol, about 28% 1,2-heptadecanediol and about 16% 1,2-octadecanediol) were charged to a glass reactor equipped with heater, agitator, Dean-Stark tube with condenser and provision for blanketing the vapor space with nitrogen. The contents were heated to 70° C. to liquify and 55 g of dimethyl hydrogen phosphite were slowly added. The reaction mixture was heated to 110° C. and held for 2 hours, held at 120° C. for 1 hour, and held at 130° C. for 1 hour. During this reaction period, methanol distilled over and condensed into the trap. The crude product was vacuum stripped at 150° C. to remove volatile materials. 379 g of finished additive were produced. The product was an amber fluid which became waxy on cooling.

Aufarbeitung

  1. customequipped with heater, agitator, Dean-Stark tube with condenser
  2. temperatureThe reaction mixture was heated to 110° C.
  3. waitheld at 120° C. for 1 hour
  4. waitheld at 130° C. for 1 hour
  5. distillationdistilled over and
  6. customcondensed into the trap
  7. customstripped at 150° C.
  8. customto remove volatile materials
  9. custom379 g of finished additive were produced
  10. temperatureon cooling

Quellen und Nachweise

ORD-Eintrag
ord-edebad08f5b148ccac7479e949a5f540
Quelldatensatz
uspto-grants-1985_07
Patentnummer
US04532057

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