Реакция #2282184

ord-1f51aaf1871a44d8b311c8bb1a062058

Условия реакции

Температура
65°CELSIUS
Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    Другоеfitted with a stirring apparatus
  2. 2
    Другоеwas performed at 110° C. under a nitrogen
  3. 3
    Другоеfor 1 hour
  4. 4
    Температураwas heated under a nitrogen stream at normal pressure to 150° C. as a reaction temperature
  5. 5
    Другоеreached 150° C.
  6. 6
    workup.WAITThe reaction time was 8 hours
  7. 7
    Фильтрацияthe product was filtrated at 80° C.

Методика

After 469 g of a 70% by weight sorbitan aqueous solution (aldehyde value of sorbitan: 6.5 ppm) and 556 g of methyl laurate were charged into a 2000 mL four-neck flask fitted with a stirring apparatus, a thermometer, and a nitrogen gas inlet, dehydration was performed at 110° C. under a nitrogen stream at normal pressure for 1 hour and further at 110° C. under a nitrogen stream at 4 kPa for 1 hour. The whole was cooled to 65° C. and, after 35.4 g of a 5% by weight sodium methoxide methanol solution and 0.44 g of sodium hypophosphite were added thereto, was heated under a nitrogen stream at normal pressure to 150° C. as a reaction temperature. After the temperature reached 150° C., the reaction was carried out under a nitrogen stream at normal pressure. At the time point when the spot of methyl laurate as a raw material disappeared on thin-layer chromatography, it was judged that the reaction was completed. The reaction time was 8 hours and, after the completion of the reaction was confirmed, the product was filtrated at 80° C. to obtain sorbitan monolaurate.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US08334397B2uspto-grants-2012_12